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EUPT – SRM13April/May 2018

EU Proficiency Test on the Analysis of Pesticides Residues

Requiring Single Residue Methods

in Soybean Flour

Chemisches und Veterinäruntersuchungsamt

Stuttgart

Final Report

EU Reference Laboratories for Residues of Pesticides Single Residue MethodsEURL-SRM

EU PROFICIENCY TESTEUPT-SRM13, 2018

Residues of PesticidesRequiring

Single Residue Methods

Test Item: Soybean Flour

Final Report Part One: Resutls Evaluation (excl. Phosphine)

Michelangelo AnastassiadesPat Schreiter

Anja BarthHubert Zipper

approved by Michelangelo Anastassiades released on 31 October, 2018

The EURL-SRM is accredited by the DAkkS according to EN ISO/IEC 17043. The accreditation is valid for the proficiency testing programs listed in the certificate.

Publication of parts of this EUPT-SRM13 final report by individuals or organizations shall always refer to the original document that can be found under: http://www.eurl-pesticides.eu/library/docs/srm/EUPT_SRM13_FinalReport.pdf

Picture on the book cover: Tharakorn Arunothai, www.shutterstock.com, 219828004

http://www.eurl-pesticides.eu/library/docs/srm/EUPT_SRM13_FinalReport.pdf

Organisers

Michelangelo Anastassiades

Head of EURL-SRM (Single Residue Methods)CVUA StuttgartDepartment of Residues and ContaminantsSchaflandstrasse 3/2D-70736 Fellbach

Phone: +49-711-3426-1124Fax: +49-711-588176E-Mail: [email protected]

Advisory Group:

Amadeo Fernández-Alba EURL-FV, University of Almería (UAL), ES

Miguel Gamón EURL-FV, Laboratorio Agroalimentario Generalitat Valenciana (LAGV), ES

Mette Erecius Poulsen EURL-CF, National Food Institute (DTU), Søborg, DK

Ralf Lippold EURL-AO, CVUA Freiburg, DE

Philippe Gros Service Commun des Laboratoires (SCL) / Laboratoire de Montpellier, FR

Magnus Jezussek Bavarian Health and Food Safety Authority (LGL), Erlangen, DE

André de Kok Netherlands Food and Consumer Product Safety Authority (NVWA), Wageningen, NL

Sonja Masselter Austrian Agency for Health and Food Safety (AGES), Innsbruck, AT

Finbarr O’Regan Pesticide Control Laboratory (PCL), Department of Agriculture, Food and the Marine, IE

Tuija Pihlström National Food Agency (Livsmedelsverket), Uppsala, SE

Patrizia Pelosi National Institute of Health (ISS), Roma, IT

Carmelo Rodríguez University of Almería (UAL), ES

Quality Control Group:

Antonio Valverde University of Almería, ES

Paula Medina European Food Safety Authority (EFSA)

Organising Team:

EURL for Pesticides Requiring Single Residue Methods hosted by CVUA Stuttgart

Pat Schreiter, Senior Food Chemist

Anja Barth, Chemical Technician

Hubert Zipper, Senior Food Chemist

Carmen Wauschkuhn, Senior Food Chemist

Eric Eichhorn, Food Chemist

Nadine Kotte, Food Chemist

Giovanna Cerchia, Chemical Technician

Dorothea Mack, Chemical Technician

Sigrid Schüler, Chemical Technician

Sahra Söhnholz, Chemical Technician

Cristin Wildgrube, Chemical Technician

EURL for Pesticides in Cereals and Feedingstuff, National Food Institute, Technical University of DenmarkJens-Ole Frimann, Software Programmer

EUPT-Coordinator:

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FOREWORD

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FOREWORD

Regulation 882/2004/EC [1] defines the general tasks and duties of the EU Reference Laboratories (EURLs) for Food, Feed and Animal Health1 including the organisation of comparative tests (proficiency tests = PTs). These PTs are carried out on an annual basis and aim to improve the quality, accuracy and comparability of the analytical results generated by EU Member States within the framework of the EU coordinated control programs as well as national monitoring programs. By participating in PTs laboratories can assess and at the same time demonstrate their analytical performance. The attention to details paid by laboratories during PT-analysis, together with the need to identify errors and to take corrective actions in cases of underper-formance, typically lead to improvements in the quality of analytical results.

According to Article 28 of Regulation 396/2005/EC on maximum residue levels of pesticides in or on food and feed of plant and animal origin [2], all laboratories analysing for pesticide residues within the frame-work of official controls shall participate in the European Union Comparative Proficiency Tests (EUPTs) for pesticide residues. Each Official Laboratory (OfL) must participate in EUPTs concerning the commodities included in its area of competence.

Since 2006 the EURL for pesticide residues requiring the use of Single Residue Methods, EURL-SRM, has an-nually conducted one scheduled Proficiency Test. Five of those thirteen EUPT-SRMs were conducted in col-laboration with the EURL for pesticide residues in Fruits and Vegetables (EURL-FV) with apple juice (EUPT-SRM1, 2006), carrot homogenate (EUPT-SRM3, 2008), apple purée (EUPT-SRM5, 2010), potato homogenate (EUPT-SRM8, 2013) and spinach homogenate (EUPT-SRM11, 2016) as test items. Further four EUPT-SRMs were conducted in collaboration with the EURL for pesticide residues in Cereals and Feeding Stuff (EURL-CF) with wheat flour (EUPT-C1/SRM2, 2007), oat flour (EUPT-C3/SRM4, 2009), rice flour (EUPT-C5/SRM6, 2011) and maize flour (EUPT-C9/SRM10, 2015) as test items. The remaining four EUPT-SRMs were organized by the EURL-SRM unilaterally, two of them used commodities from plant origin with low fett content : milled dry lentils (EUPT-SRM7, 2012) and soybean slour (EUPT-SRM12, 2017). The EUPT-SRM9 was the only EUPT-SRM so far, in which a commodity of animal origin (cow’s milk) was used. The current PT using flour of whole soybeans was the first one using a commodity with low water and high oil content (approx. 22 %).

Participation in the respective EUPTs is mandatory for all NRLs for pesticides requiring Single Residue Meth- ods (NRL-SRMs) and for all OfLs analysing pesticide residues within the framework of national or EU control programs in commodities represented by the respective EUPT test item. Laboratories in EU Member States analysing pesticide residues within the frame of import controls according to Reg. 669/2009/EC are also considered as performing official controls in the sense of Reg. 882/2005/EC and 396/2005/EC and are thus also obliged to take part in EUPTs. OfLs from EFTA countries (Iceland, Norway and Switzerland) contributing data to the EU-coordinated community control programs, EU laboratories analysing official organic samples within the frame of Reg. 889/2008/EC, as well as OfLs from EU-acceding or -candidate countries (FYROM, Montenegro, Serbia and Turkey) are also invited to take part. A limited number of laboratories from third countries are allowed to take part in this exercise, too. However, only results submitted by labs from EU and EFTA countries are included in the calculation of the assigned values. In order to have sufficient results for evaluation of phosphine, a few private laboratories were exceptionally invided to participate in the present PT. These private labs were also allowed to report results also for any other pesticides in the target pesti-cides list, but those results was neither used to establish the assigned values nor be presented in this report.

1 Formerly known as Community Reference Laboratories (CRLs)

Based on information about the commodity scope and labs’ NRL-status a tentative list of EU-labs consid-ered as being obliged to participate in the EUPTs is published at the beginning of each year. The pesticide scope is not taken into account in these lists. NRLs and OfLs listed as being obliged to participate in an EUPT exercise in a given year but deciding not to take part, are always asked to state the reason(s) for their non-participation. The same applies to laboratories originally registering to participate in a certain EUPT but finally not submitting results.

DG-SANTE has full access to all data of EUPTs including the lab-code/lab-name key. The same applies to all NRLs as far as laboratories belonging to their own country networks are concerned. Results for this EUPT or a series of EUPTs, evaluated on a country by country basis, may be further presented to the European Commission Standing Committee on Plants, Animals, Food and Feed (PAFF)-Section Pesticides Residues ,or during the EURL-Workshops.

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CONTENT

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CONTENT

FOREWORD ................................................................................................................................................................................v

INTRODUCTION ..................................................................................................................................................................ix

1. TEST ITEM AND BLANk MATERIAL ..............................................................................................1

1.1 Selection of PT-Commodity and of Compounds for the Target Pesticides List ................1

1.2 Small Scale Preliminary Investigation on Analytes during Homogenisation ...................1

1.3 Preparation and Bottling of the Blank Material ......................................................................................2

1.4 Preparation and Bottling of the Blank Material ......................................................................................2

1.5 Packaging and Delivery of PT Materials to Participants ..................................................................3

1.6 Analytical Methods ........................................................................................................................................................3

1.7 Homogeneity Test ..........................................................................................................................................................4

1.8 Storage Stability Test ..................................................................................................................................................5

1.9 Transport Stability Test .............................................................................................................................................7

1.10 Organisational Aspects ..............................................................................................................................................8

2. EVALUATION RULES ........................................................................................................................................11

2.1 False Positives and Negatives ..............................................................................................................................11

2.2 Assigned Values (xpt) and Calculation of the Respective Uncertainties (u(xpt)) .............11

2.3 Fixed Target Standard Deviation using FFP-Approach (FFP-σpt) .............................................. 12

2.4 z-Scores ............................................................................................................................................................................... 12

2.5 Laboratory Classification ...................................................................................................................................... 12

3. PARTICIPATION ................................................................................................................................................. 15

4. RESULTS ......................................................................................................................................................................... 19

4.1 Overview of Results ................................................................................................................................................... 19

4.2 Analysis of Blank Material .....................................................................................................................................30

4.3 Assigned Values and Target Standard Deviations .............................................................................30

4.4 Assessment of Laboratory Performance ................................................................................................... 32

5. ACkNOWLEDGEMENTS ............................................................................................................................. 53

6. REFERENCES ............................................................................................................................................................. 53

EUPT-SRM13 | 2018 (Soybean Flour)

viii

7. APPENDICES .......................................................................................................................................................... A-1

Appendix 1 ................. List of Laboratories Registered to Participate in the EUPT-SRM13 A-1

Appendix 2 ................. Shipment Evaluation .........................................................................................................A-5

Appendix 3 ................. Data of Homogeneity Test ...........................................................................................A-6

Appendix 4 ................. Data of Stability Test ........................................................................................................A-8

Appendix 5 ................. Histograms and kernel Density Estimates of z-score Distributions A-11

Appendix 6 ................. Graphic Presentation of z-Scores ........................................................................... A-13

Appendix 7 ................. Possible Reasons Reported for Poor Performance ..................................A-26

Appendix 8 ................. General EUPT Protocol (8th Ed.) ...............................................................................A-39

Appendix 9 ................. Specific Protocol of EUPT-SRM13 ...........................................................................A-47

Appendix 10 ............... Calendar and Target Pesticides List of EUPT-SRM13 ...............................A-51

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INTRODUCTION

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european CommIssIon – eu-proFICIenCy test on resIdues oF pestICIdes

requIrIng sIngle resIdue methods

test Item: soybean Flour

EUPT-SRM13, 2018

INTRODUCTION

On 23 Januar, 2018 all relevant National Reference Laboratories (NRLs) of the 28 EU-Member States (MS), as well as all relevant EU-Official Laboratories (OfLs) whose contact details were available to the organis-ers (EURL-SRM) were invited to participate in the 13th European Commission‘s Proficiency Test Requiring Single Residue Methods (EUPT-SRM13). The EUPT-SRM13-Website contained links to the Announcement/Invitation Letter, the Calendar, as well as to the Target Pesticides List (see Appendix 11). The Target Pesti-cides List contained 25 compounds potentially being present in the test item. 9 of them were compulsory compounds and were thus considered in the Category A/B classification (based on scope). The compounds of the Target Pesticides List were selected based on a number of criteria and following consultation with the EUPT-Scientific Committee. For each compound a residue definition valid for the PT and the minimum required reporting level (MRRL) were stipulated. Links to the latest version of the “General Protocol” (see Appendix 9) containing information common to all EUPTs and to the “Specific Protocol” (see Appendix 10) valid for the current PT were also provided. The laboratories were able to register on-line from 27 February to 16 March, 2018.

Based on its commodity scope (fruit and vegetables, feed, and commodities with high fett content) and its NRL-status (NRL-SRMs) a tentative status of a laboratory to be obliged to participate in the EUPT-SRM13 was stored in the DataPool, so that every participant can see it during the registration. To ensure that all relevant official laboratories were informed about this EUPT, the NRLs were asked to forward the invitation to all relevant official laboratories within their countries. It was made clear that the status of the labora-tories was only tentative, and the real obligation to participate was based on Reg. 396/2005/EC and Reg. 882/2004/EC. Obliged labs that did not intend to participate were asked to provide an explanation.

In total 114 participating labs from EU and EFTA countries, 2 OfLs from an EU candidate country and 8 labo-ratories from third countries submitted results of at least one compound. Except 5 laboratories from EU and EFTA countries all other registered laboratories have submitted results.

The proficiency test EUPT-SRM13 was conducted using organic soybean flour originated from Austria and organic soybeans from EU countries. The test item was prepared by spiking the soybeans with 15 com-pounds highly concentrated dissolved in standard solutions, milling, filtering and mixing with the organic soybean flour. More details are given in Chapter 1 “Test Materials and Blank Material”.

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1. TEST ITEM / Selection of PT-Commodity and of Compounds for the Target Pesticides List

1. TEST ITEM AND BLANk MATERIAL

1.1 Selection of PT-Commodity and of Compounds for the Target Pesticides List

In agreement with the EUPT- Scientific Committee soybean flour was chosen as commodity for the EUPT-SRM13.

The compounds to be included in the Target Pesticides List (Appendix 11) were selected by the organiser and the EUPT-Scientific Committee (Advisory Group and Quality Control Group) taking the following points into account: 1) the present and upcoming scope of the EU-coordinated control program; 2) a pesticide pri-ority list, ranking the pesticides according to their risk potential; 3) the relevance of pesticides to the specific commodity; 4) the overall scope and capability of the OfLs as assessed in previous PTs or surveys.

For the production of the test item and the blank material, one batch of organic soybean flour were pur-chased from a food processing company and checked for the absence of the analytes on the Target Pesti-cides List. None of the target pesticides was detected except phosphonic acid at 0.04 mg/kg and bromide ion at 1.3 mg/kg. More soybean flour of the same batch was purchased. This batch was finally used for the preparation of the blank material and for the preparation of the test item by spiking with 15 compounds (see Section , p. 3).

The minimum required reporting levels (MRRLs) were set at 0.003 mg/kg for haloxyfop; at 0.005 mg/kg for carbofuran and phosphine; at 0.01 mg/kg for 2,4-D, chlormequate-Cl, cyromazine, fluazifop, mepiquat-Cl, 2,4-DB, chlorate, fenoxaprop, perchlorate and quizalofop; at 0.02 mg/kg for ethephon, bentazone, diquat, glufosinate, MPP, N-acetyl glufosinate, and N-acetyl glyphosate, and paraquat; at 0.03 mg/kg for glypho-sate; at 0.05 mg/kg for AMPA and phosphonic acid and at 2.0 mg/kg for bromide ion.

1.2 Small Scale Preliminary Investigation on the Behavior of the Analytes during Ho-mogenisation

In order to estimate the loss of spiked analytes during the preparation of the test material, several preliminary spiking experiments were performed at a small scale.

1.2.1 Recovery Study

A recovery study (n = 5) for all analytes listed on the Target Pesticides List was conducted. Recover-ies were found to be (65 %) 93 – 117 %.

1.2.2 Investigation on Homogeneity and on the Behavior of Analytes during Test Material Prepa-ration using soybean flour in comparison with soybeans

The experiments consisted of spiking one portion (100 g) of soybean flour and one portion (100 g) of soybeans with a representative selection of pesticides listed on the Target Pesticides List as a mixture. The spiking was conducted in a metallic container. The spiked soybeans were dried and afterwards ground in a Thermomix® adding dried ice. The test materials both prepared with soybean flour and soybean were homogenized with blank soybean flour 1:10. These small scale test materials were analyzed for the yield of all spiked analytes using QuEChERS method and QuPPe PO method (n = 7).


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Results showed that with the test material prepared with soybean flour acceptable yields (86 % – 109 %) could be obtained. However the results for homogeniety were not satisfying (RSD 22 % – 30 %)

Test material which was prepared with soybeans homogenized with soybean flour, obtained yields showed acceptable results for some analytes but also very low yields (37 % – 38 %) especially in case of highly polar pesticides. Here results for homogeniety were satisfying (RSD 4 % – 15 %).

It was concluded that another test is needed where the spiking of soybeans is conducted in a plastic container.

1.2.3 Investigation on the Behavior of Analytes during Test Material Preparation using Soybeans

1 kg soybeans was spiked with a representative selection of pesticides listed on the Target Pesticides List as a mixture. The spiking was conducted in a plastic container. The spiked soybeans were dried and afterwards ground in a Thermomix adding dried ice. This small scale test material was analyzed for the yield of all spiked analytes using QuEChERS method and QuPPe PO method (n = 4).

Yields obtained with the test material which was prepared in a plastic container showed satisfying results ((65 %) 90 – 119 %) and also satisfying homogeneity (RSD 2 % – 12 % (26 %)).

Using soybeans for spiking (in a plastic container) followed by dilution and homogenization with soybean flour was considered appropriate for the preparation of the test item.

1.3 Preparation and Bottling of the Blank Material

Treatment of blank soybeans was conducted to obtain the same conditions present in the sample material.

2.5 kg soybeans were spiked with a solvent mixture which corresponded both in volume and composition to the spiking solution (see below). These soybeans were dried and ground in a Thermomix® adding dry ice. Approximately 50 kg organic soybean flour from 5 packages, each containing 20 kg, were pooled in a large metal vessel, where it was layered with the processed blank soybeans. The blank material was mixed with a drum-hoop mixer over 10 h. Approximately 200 g portions of the well-mixed blank soybean flour were weighed out into labelled and leak-proof screw-capped polyethylene plastic bottles, sealed and stored in a freezer at about −20 °C until distribution to participants.

1.4 Preparation and Bottling of the Blank Material

The test item was prepared in the same way as the blank material described above, but instead of adding pure solvent 150 ml of an equally composed mixture containing the target analytes was added. The mixture contained 14 different compounds and was prepared as described in Table 1-1 (p. 3)..

These two processed soybean flours and approximately 50 kg organic soybean flour from 5 packages were layered, and pooled in a large metal vessel. The spiked material was mixed with a drum-hoop mixer over 10 h. Approximately 200 g portions of the well-mixed spiked soybean flour were weighed out into labelled and leak-proof screw-capped polyethylene plastic bottles, sealed and stored in a freezer at about −20 °C until distribution to participants.

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1. TEST ITEM and Blank Material / Investigation on Analysis of Carbofuran and Bifenazate

1.5 Packaging and Delivery of PT Materials to Participants

Three days prior to the sample delivery, one bottle of test item and one of blank material, both deep frozen, as well as were packed into thermo-insulated polystyrene boxes, filled with four cooling elements and stored at −20 °C for three days, so that at the day of delivery the cooling elements were deep frozen. Once the parcel was picked up by DHL, the recipient received an e-mail from the shipping company entailing the individual online tracking number.

Among the 122 packages sent to laboratories in EU and EFTA countries, 106 (87 %) reached the participating labs within 24 hours and 11 packages within 48 hours. Due to the remote location of certain laboratories and holidays in certain countires, the remaining 5 packages took 3 days to arrive. The delivery to countries outside the EU and EFTA zones was accomplished within 48 hours in 3 cases, within 72 hours in 2 cases, within 4 days in 1 case, and more than 7 days in 4 cases. The latter was, however, due to delays at the customs. Overall, the EUPT-materials arrived at the laboratories very cold within two days. All material was accetped by the participants. Details on the shipment duration are shown in Appendix 2.

At this point organisers would like to appeal to the participants to follow their own parcels via the online tracking tool of the shipping company in order to maintain the ability to take the necessary measures in case of delays, e.g., contacting the customs to ask for an acceleration of the clearance procedure or to place the parcel in a cool place until clearance is granted. The participants are furthermore encouraged to con-tact the local office of the shipping company to ensure optimal delivery in case of opening time.

1.6 Analytical Methods

The analytical methods used by the organisers to check the homogeneity and storage-stability of the target analytes contained in the test item as well as the absence of target analytes in the blank material are summarized in Table 1-2 (p. 4). For more details on the methods used, please refer to the EURL-SRM website: http://www.eurl-pesticides.eu (EURL-SRM-website Services Methods).

Table 1-1: Analytes spiked into 50 kg soybean flour for the preparation of the test material

Analytes dissolved in 50 ml H2O Theor. Conc. Analytes dissolved in 100 ml Aceton Theor. Conc.

Compound Amount [mg/kg] Compound Amount [mg/kg]

Bromide-K 1097.84 mg 14.742 1) 2,4-DB 10.238 mg 0.205

Cyromazine 5.64 mg 0.113

Glyphosate 50.27 mg 1.005

Mepiquat-Cl 6.8 mg 0.136

Perchlorate-Na 6.473 mg 0.105 2)

Diquat-dibromid hydrate 152.203 mg 1.549 3) Spiking using Stock Solution (1 mg/ml ACN) Theor. Conc.

Glufosinate-Al 11.098 mg 0.203 4) Compound Amount [mg/kg]

MPPA 8.826 mg 0.177 Haloxyfop (free acid) 0.8 ml 0.016

N-Acetyl-glyphosate 30 mg 0.600 Fluazifop (free acid) 2.6 ml 0.052

Phosphonic acid 103.064 mg 2.061 Quizalofop (free acid) 3.0 ml 0.060

1) as bromide ion; 2) as perchlorate; 3) as diquate dication; 4) as glufosinate

http://www.eurl-pesticides.eu


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1.7 Homogeneity Test

After filling the test item in the bottles, 10 bottles were randomly chosen for the homogeneity test and two analytical portions were taken from each for analysis. Both the order of sample preparation and the order of extract injection into the analytical instruments were random. Matrix-matched calibration using extract prepared from blank material or procedural calibration using blank material were applied for quantifica-tion. Analytical portions of 1 g for phosphine and 5 g for all other compounds were used.

Table 1-2: Analytical methods used by the organisers to check for the homogeneity and storage-stability of the pesticides present in the test item and to demonstrate the absence of other pesticides in the blank material.

Compound Extraction IS Determinative analysis Notes

2,4-DB Modified QuEChERS-method [3] involving: weighing of 5 g soybean flour into a sealable vessel, addition of 10 ml H2O, extraction with ACN (15 min), addition of partitioning salts (4 g MgSO4, 1 g NaCl, 1 g trisodium citrate dihydrate and 0.5 g disodium hydrogenci-trate sesquihydrate), 1 min shaking, centrifugation, addition of IS / ILISs to raw extract and direct determination by LC-MS/MS in the ESI (neg.) and ESI (pos) mode.

BNPU LC-MS/MS ESI (neg)

Fluazifop BNPU LC-MS/MS ESI (neg)

Haloxyfop BNPU / Haloxyfop D4 LC-MS/MS ESI (neg)

Quizalofop BNPU / Quizalofop D3 LC-MS/MS ESI (neg)

2,4-D* BNPU LC-MS/MS ESI (neg)

Bentazone* BNPU LC-MS/MS ESI (neg)

Carbofuran* Chlorpyrifos D10 LC-MS/MS ESI (pos)

Fenoxaprop* BNPU LC-MS/MS ESI (neg) –

Bromide ion QuPPe-PO method [5] involving: weighing of 5 g soybean flour into a sealable vessel, addition of ILISs, addition of methanol containing 1 % formic acid, shaking, centrifugation, Filtration, cleanup with C18 and pos-sibly dilution with MeOH containing 1 % formic acid. Determination by LC-MS/MS in the ESI (neg.) or ESI (pos.) mode.

– LC-MS/MS ESI (neg) QuPPe M1.3

Cyromazine Cyromazine D4 LC-MS/MS ESI (pos) QuPPe M4.2

Glufosinate Glufosinate D3 LC-MS/MS ESI (neg) QuPPe M1.3

Glyphosate Glyphosate 13C 15N LC-MS/MS ESI (neg) QuPPe M1.3

Mepiquat Mepiquat D3 LC-MS/MS ESI (pos) QuPPe M4.2

MPP MPP D3 LC-MS/MS ESI (neg) QuPPe M1.3

N-Acetyl-Glyphosate N-Acetyl-Glyphosate 13C2

15NLC-MS/MS ESI (neg) QuPPe M1.3

Perchlorate Perchlorate 18O4 LC-MS/MS ESI (neg) QuPPe M1.4

Phosphonic acid Phosphonic acid 18O3 LC-MS/MS ESI (neg) QuPPe M1.4

AMPA* AMPA 13C 15N LC-MS/MS ESI (neg) QuPPe M1.3

Chlorate* Chlorate 18O3 LC-MS/MS ESI (neg) QuPPe M1.4

Chlormequat* Chlormequat D4 LC-MS/MS ESI (pos) QuPPe M4.2

Ethephon* Ethephon D4 LC-MS/MS ESI (pos) QuPPe M4.2

N-Acetyl-Glufosinate* N-Acetyl-Glufosinate D3 LC-MS/MS ESI (neg) QuPPe M1.3

Paraquat* Paraquat D6 LC-MS/MS ESI (pos) QuPPe M4.1

Diquat QuPPe-PO method [5] involving: weighing of 5 g soybean flour into a sealable vessel, addition of ILIS, addition a 1:1 mixture of methanol+ aqueous HCl 0.1 M, shaking, centrifu-gation, Filtration, cleanup with C18 and determination by LC-MS/MS in the ESI (pos.) mode.

Diquat 13C2 LC-MS/MS ESI (pos) QuPPe M4.1

Phosphine xxxxxxxxxxxxxxxxxx H2S GC-MS EI (pos)

* : To check for absence in Blank Material

1. TEST ITEM and Blank Material / Storage Stability Test

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The statistical evaluation of the homogeneity test data was performed according to the International Har- monized Protocols published by IUPAC, ISO and AOAC [4, 6]. An overview of the statistical evaluations of the homogeneity test is shown in Table 1-3. The individual residue data of the homogeneity test is given in Appendix 3.

The acceptance criterion for the test item to be sufficiently homogeneous for the Proficiency Test was that ssam

2 is smaller than c with ssam being the between-bottle sampling standard deviation and c = F1 × σall

2 + F2 × san2, F1 and F2 being constants with values of 1.88 and 1.01, respectively, and applying

when duplicate samples are taken from 10 bottles. σall2 = 0.3 × FFP-RSD (25 %) × the analytical sampling

mean of the analyte, and san is the estimate of the analytical standard deviation.

As all target compounds passed the homogeneity test, the test item was considered to be sufficiently ho-mogenous and suitable for the EUPT-SRM13.

1.8 Storage Stability Test

In the Specific Protocol laboratories were recommended storing the samples in the freezer until analysis. The stability test samples were thus also stored under the same conditions. Shortly after the shipment of the samples to the participants, three of the spare test item bottles were chosen randomly and all analyti-cal portions necessary for all three stability tests were weighed into the vessels in which the analysis was

COMPULSORY COMPOUNDS

Brom

ide

ion

Cyro

maz

ine

Flua

zifo

p

free

aci

d

Gly

phos

ate

Hal

oxyf

op

free

aci

d

Mep

iqua

t-Cl

Analytical portion size [g] 5 5 5 5 5 5

Mean [mg/kg] 14.6 0.107 0.049 0.924 0.016 0.126

ssam2 2.34 × 10-1 6.76 × 10-6 2.73 × 10-6 4.58 × 10-4 4.34 × 10-8 2.82 × 10-5

c 3.30 × 100 1.62 × 10-4 2.89 × 10-5 1.27 × 10-2 3.27 × 10-6 2.15 × 10-4

Passed/Failed passed passed passed passed passed passed

Table 1-3: Statistical evaluation of homogeneity test data (n = 20), details please see Appendix 3.

OPTIONAL COMPOUNDS

2.4-

DB

fr

ee a

cid

Diq

uat

dica

tion

Glu

fosi

-nat

e

MPP

N-A

cety

l-G

lyph

osat

e

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

free

aci

d

Phos

phin

e (t

est I

tem

)

Phos

phin

e (P

H3-

Tube

)

Analytical portion size [g] 5 5 5 5 5 5 5 5 1 1

Mean [mg/kg] 0.177 1.46 0.197 0.175 0.759 0.103 1.99 0.058 0.168 0.068

ssam2 1.44 × 10-5 3.41 × 10-3 2.25 × 10-4 5.90 × 10-5 1.79 × 10-3 3.91 × 10-6 7.33 × 10-3 2.06 × 10-6 2.34 × 10-7 0 × 10-0

c 4.11 × 10-4 3.44 × 10-2 8.71 × 10-4 4.19 × 10-4 8.58 × 10-3 1.48 × 10-4 5.46 × 10-2 4.24 × 10-5 8.71 × 10-8 1.14 × 10-4

Passed/Failed passed passed passed passed passed passed passed passed passed passed


6

to be conducted. The portions of stability tests 1 were extracted immediately and those of stability tests 2 and 3 were placed in the freezer at −20 °C until analysis as described in Section 1.6 (p. 3). The extracts of all stability tests corresponding to one method were stored in the freezer at −20 °C and measured iso-chronically (within the same sequence) at a day suitable for the laboratory.

Stability test 1 (extraction shortly after shipment): 03 May 2018 (analytes via QuPPe-Methods) 25 April 2018 (analytes via QuEChERS-Methods) 28 May 2018 (phosphine (PH3-Tube)) 20 June 2018 (phosphine (test item))

Stability test 2 (extraction five weeks or more after shipment): 22 May 2018 (analytes via QuPPe-Methods) 17 May 2018 (analytes via QuEChERS-Methods) 19 June 2018 (phosphine (PH3-Tube)) 19 July 2018 (phosphine (test item))

Stability test 3 (extraction at least four weeks after deadline for results submission): 18 June 2018 (analytes via QuPPe-Methods) 07 June 2018 (analytes via QuEChERS-Methods) 18 July 2018 (phosphine (PH3-Tube)) 24 Sept. 2018 (phosphine (test item))

A target compound is considered to be adequately stable if |yi − y| ≤ 0.3 × σpt, where yi is the mean value of the last period of the stability test, y is the mean value of the first period of the stability test and σpt the standard deviation used for proficiency assessment, typically 25 % of the assigned value. With the excep-tion of phosphine all other analytes contained in the test item showed a stability within the acceptable limits when stored under the recommended conditions (−18 °C) within a period exceeding the duration of the exercise by two weeks (Table 1-4, p. 7). For the compounds passing the test it is assumed that, if the recommended storage conditions were followed, the influence of sample storage on the results of these analytes was negligible at least throughout the duration of the EUPT.

In the case of phosphine (PH3-Tube) the determined concentration in day 3 was lower than that deter-mined in day 1 by 20.0 %. This decline was significantly higher than the tolerance of 8.725 % (= 0.3σpt us-ing FFP-RSD of 25 %). In case of phosphine (PT-Sample), compared with the concentration on day 1, the determined concentration in day 3 declined only 4.25 %. However, the determined concentration in day 2 deviated by 17.29 % that was higher than the tolerance of 0.3σpt.

This fluctuation of the results of the stability test and the broad standard diviation reflected the fact that the analytical method was not robust. The analytical results of phosphine is thus associated with a considerable uncertainty. The determined deviations are probably related more to spurious analytical errors rather than to degradation. The higher concentration in day 2 compared to day 1 also points towards this direction. As analysis of phosphine is an optional compound in the PT, no further measures concerning its stability were deemed necessary, but report will be issued separately for its evaluation.

The results of all analyses conducted within the framework of the stability test are shown in Table 1-4 and Appendix 4.

1. TEST ITEM and Blank Material / Transport Stability Test

7

TesT

ITem

1

Table 1-4: Results of storage stability test (storage at -18 ºC). Please see the text or Appendix 4 for the dates of analysis for each analytes.


Brom

ide

ion

Cyro

maz

ine

Flua

zifo

p

free

aci

d

Gly

phos

ate

Hal

oxyf

op

free

aci

d

Mep

iqua

t-Cl

Storage at −18 ºC (mean values in mg/kg)

Analysis 1 13.729 0.105 0.050 0.913 0.016 0.123

Analysis 2 14.054 0.105 0.050 0.964 0.016 0.128

Analysis 3 14.110 0.111 0.049 0.933 0.017 0.131

Deviation [mg/kg] ([%]) Analysis 3 vs. Analysis 1

0.381 (2.8 %)

0.006 (5.3 %)

0.001 (-1.7 %)

0.02 (2.2 %)

0.001 (7.1 %)

0.008 (6.2 %)

0.3 × σpt [mg/kg] 1.152 0.007 0.004 0.068 0.001 0.009

Passed/Failed passed passed passed passed passed passed


2.4-

DB

fr

ee a

cid

Diq

uat

dica

tion

Glu

fosi

-nat

e

MPP

N-A

cety

l-G

lyph

osat

e

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

free

aci

d

Phos

phin

e (t

est I

tem

)

Phos

phin

e (P

H3-

Tube

)

Storage at −18 ºC (mean values in mg/kg)

Analysis 1 0.177 1.423 0.186 0.170 0.734 0.101 1.922 0.058 0.180 0.063

Analysis 2 0.183 1.359 0.183 0.174 0.773 0.101 1.959 0.059 0.149 0.069

Analysis 3 0.165 1.422 0.186 0.165 0.742 0.108 1.939 0.058 0.188 0.080

Deviation [mg/kg] ([%]) Analysis 3 vs. Analysis 1

0.012 (-7.0 %)

0.001 (-0.1 %)

0 (0 %)

0.004 (-2.6 %)

0.008 (1.1 %)

0.007 (6.5 %)

0.016 (0.9 %)

0.001 (-1.2 %)

0.008 (4.25 %)

0.013 (20.0 %)

0.3 × σpt [mg/kg] 0.014 0.128 0.014 0.014 0.063 0.007 0.140 0.004 0.007 0.003

Passed/Failed passed passed passed passed passed passed passed passed passed failed

1.9 Transport Stability Test

With the exception of 7 laboratories with remote location or being on holiday and further 5 laboratories where the shipments were retarded due to customs clearance delays or remote location, all other 120 laboratories (91 %) received their test items within 48 hours. Among these 120 laboratories 106 received the parcels within one day. As no significantly negative influence of the long transport duration on the results from the 12 laboratories receiving the parcels more than 72 hours upon shipment was detected, the organisers decided not to conduct the transport stability test in the current PT.


8

1.10 Organisational Aspects

1.10.1 Laboratory Status as Mandatory to Participation

Based on available information on NRL-status and commodity scope as recorded in the EURL-DataPool, the EU and EFTA OfLs and NRLs are designated as "mandatory to participate in the current PT" or "participation on voluntary basis". The available information on the pesticide scope covered by the laboratories was not considered due to concerns that might not be up-to-date and/or not applicable to the present commod-ity (soybean). The OfLs can provide the organisers and their NRLs their reasons and ask for changing their status. The NRLs were reminded of their responsibility for their network and to ensure that all obliged OfLs within their network were informed of this EUPT. All NRLs and OfLs were informed that the status of obli-gation was tentative and the real obligation for participation is deriving from Art. 28 of Reg. 396/2005/EC (for OfLs) and Art. 33 of Reg. 882/2004/EC (for NRL-SRMs). Following DG-SANTE instructions, obliged labs that were not intending to participate in the EUPT-SRM13 were instructed to provide explanations for their non-participation.

1.10.2 Announcement / Invitation and EUPT-SRM13-Website

Within the EURL-Web-Portal an EUPT-SRM13-Website was constructed with links to all documents relevant to this EUPT (i.e., Announcement/Invitation Letter, Calendar, Target Pesticides List, Specific Protocol and General EUPT Protocol). These documents were uploaded to the EURL-Web-Portal and the CIRCA BC.

The Announcement/Invitation Letter for the EUPT-SRM13 was published on the EUPT-SRM13-Website in January 2018 and was sent to all NRL-SRMs, all OfLs analysing pesticide residues in food and feeding stuff within the framework of official controls, all laboratories performing import controls according to Reg. 669/2009/EC, as far as they were tracked in the EURL-DataPool, as well as to EU laboratories analys-ing official organic samples within the frame of Reg. 889/2008/EC. The latter laboratories were considered eligible but not obliged to participate. It was indicated to the OfLs that their obligation to participate in EUPTs arises from Reg. 396/2005/EC, irrespective of the content of the tentative list of obliged laboratories. NRLs and OfLs from EFTA and EU-candidate countries were also invited if their contact data was available. A number of laboratories from third countries were also invited to take part in this exercise. The acceptance of their registration was decided, however, on a case by case basis, and the laboratories were informed in-dividually of the acceptance or rejection of their registration. Furthermore, in order to obtain sufficient data for statistical evaluation of phosphine, a few private laboratories were exceptionally invited to participate in the current PT. These private laboratories were allowed to submitted also results for other analytes. However, their results for other analytes were neither be included in the establischmen of the assigned values nor present in the final report.

1.10.3 Registration and Confidentiality

Like in the previous PT in 2017 (EUPT-SRM12) the participants were able to register for this EUPT via a web-site connected to the EURL-DataPool. All laboratories being obliged to participate in the current EUPT, re-gardless of whether they were intending to participate in this exercise or not, were requested to either register or to state their reasons for non-participation using the same website.

1. TEST ITEM and Blank Material / Organisational Aspects

9

TesT

ITem

1

Upon registration or change of registration status, the labs received an electronic confirmation about their participation or non-participation in the current PT. Three days before sample shipment, participating laboratories were provided via e-mail with a unique laboratory code as well as the login data to access the online Result-Submission-Website. This ensured confidentiality throughout the entire duration of the PT.

For further information on confidentiality please refer to the General EUPT Protocol (Appendix 9).

1.10.4 Distribution of the Test Items and the Blank Material

One bottle of test item (approx. 200 g), one bottle of blank material (approx. 200 g) were shipped on 23 April, 2018 to each participant in thermo-insulated polystyrene boxes with cooling pads. All the parcels hve been precooled at -20 °C for three days before shipment.

Two weeks prior to the shipment, detailed instructions on how to treat the test item and blank material upon receipt were provided to the participating laboratories in the Specific Protocol (Appendix 10).

1.10.5 Submission of Results and Additional Information

An online submission tool allowed participants to submit their results via the Internet. Using their individ-ual login data, all participants had access to the Result-Submission-Website from a week after the sample shipment until the result submission deadline (30 May 2018). Participants were asked not only to report their analytical results but also to state whether the compounds on the Target Pesticides List were part of their routine scope and to indicate their experience with the analysis of these compounds. In addition, laboratories had to provide details about the methods applied and to state their own reporting limits (RLs) for each target compound they had analysed. The participants had furthermore the possibility to make statements as regards the condition of the material received. This information could be submitted from the day of shipment onwards.

1.10.6 Actions following Results Submission and Distribution Preliminary Report

Where information on analytical methods or results was inconsistent, laboratories were contacted. Labo-ratories that had originally registered to participate in the current PT but finally did not submit any results, were asked to provide explanations. On 19 June, 2018, the preliminary report on the EUPT-SRM13 with the preliminary assigned values was released and sent to the participants. Laboratories having submitted false positive or negative results were asked to provide information on the methods used for analysing those compounds. In addition, participants were asked to investigate the reasons for results with | z-score | > 2 and to report them. In order to have the complete and correct data for the evaluation, a reminder was sent to the participants again to fill in all the data requested on the submission page for the methodological information.

In order to obtain feedback from the participants and to improve the service quality in the future, the proofreading version of this final report (part one: results evaluation) is accompanied by a survey on EUPT-SRM13. This survey contains 5 questions on the organisation (general, registration, information and instruc-tion provided, shipment/delivery, test item, blank material and results submission pages), on the relevance of the used matrix (soybean flour) to the routine work, on the assigned values of the analytes, as well as on the preliminary report and wishes as regards the commodities and/or analytes to be included in the upcoming two EUPT-SRMs. The survey evaluation and compilation of comments will be published soon.

2. EVALUATION RULES / False Positives and Negatives

11

Eva

luat

ion

Ru

lE

2

2. EVALUATION RULES

2.1 False Positives and Negatives

2.1.1 False Positives (FPs)

Any reported result with a concentration at or above the Minimum Required Reporting Level (MRRL) of an analyte in the Target Pesticides List which was (a) not detected by the organiser, even following repetitive analysis, and/or (b) not detected by the overwhelming majority (e.g. > 95 %) of the participants that ana-lysed for this compound, is treated as a false positive result. Results of an analyte absent in the test item but with a value lower than the MRRL are excluded by the organiser and not considered as false positives. No z-scores are calculated for false positive results.

2.1.2 False Negatives (FNs)

These are results of target analytes reported as “analysed” but without reporting numerical values, al-though they were used by the organiser to prepare the test item and were detected, at or above the MRRL, by the organiser and the overwhelming majority of the participating laboratories. In accordance with the General Protocol z-scores for false negatives are calculated using the MRRL as the result, or using the lab’s reporting-limit (RL), if this is lower. Any RLs that are higher than the MRRL are not taken into account. Fol-lowing the General Protocol, results reported as “< RL” without providing a numerical value are also judged as false negatives if the RL exceeds the MRRL.

2.2 Assigned Values (xpt) and Calculation of the Respective Uncertainties (u(xpt))

In accordance with EUPT-General Protocol (Appendix 8) the assigned values xpt of each pesticide in the PT is established using the mean value of robust statistics using Algorithms A (x*) [6] of all reported results from EU and EFTA countries. Results associated with obvious mistakes and gross errors may be excluded from the population for the establishment of the assigned values. The add-in “RobStat” provided by Royal Society of Chemistry was used to calculate the assigned values with the convergence criterion = 10-6.

The uncertainty of the assigned values of each analyte is calculated according to ISO 13528:2015 [6] using the following equation:

u(xpt) = 1.25 × [(s*)/ p ]

Where u(xpt) is the uncertainty of the assigned value in mg/kg, s* is the robust standard deviation estimate in mg/kg and p is the number of data points considered (= the number of results used to calculate the assigned value). The factor 1.25 is based on the standard deviation of the median, or the efficiency of the median as an estimate of the mean, in a large set of results drawn from a normal distribution.

The tolerance for the uncertainty of the assigned value of each pesticide is calculated as 0.3 × FFP-σpt, where FFP-σpt is the target standard deviation of the assigned value derived using a fixed standard deviation of 25 % (see Section 2.3). If u(xpt) < 0.3 × FFP-σpt, is met, then the uncertainty of the assigned value is consi-dered to be negligible and not needed to be considered in the interpretation of the proficiency test results.


12

2.3 Fixed Target Standard Deviation using FFP-Approach (FFP-σpt)

Based on experience from previous EU Proficiency Tests on fruit and vegetables and cereals, the EUPT-Sci-entific Committee agreed to apply a fixed fit-for-purpose relative standard deviation (FFP-RSD) of 25 % for calculating the z-scores. The fixed target standard deviation using the fit-for-purpose approach (FFP-σpt), for each individual target analyte is calculated by multiplying the assigned value by the FFP-RSD of 25 %. In addition, the robust relative standard deviation of the assigned value (CV*) is calculated for informative purposes.

2.4 z-Scores

For each combination of laboratory and target analyte a z-score is calculated according to the following equation:

zi = (xi – xpt) / FFP-σpt

Where − xi is the result for the target analyte (i) as reported by the participant

(For results considered as false negatives, xi is set as equal to the respective minimum required reporting level (MRRL) or the laboratory reporting level (RL), if RL < MRRL.)

− xpt is the assigned value for the target analyte (i) − FFP-σpt is the standard deviation for proficiency assessment using the fit-for-purpose approach

(see above).

Any z-scores > 5 are set at 5 in calculations of combined z-scores (see 2.5.2).

The z-scores are classified as follows:

|z| ≤ 2 acceptable 2 < |z| < 3 questionable |z| ≥ 3 unacceptable

For results considered as false negatives, z-scores are calculated using the MRRL or the RL, if RL < MRRL. No z-scores are allocated to false positive results.

2.5 Laboratory Classification

2.5.1 Category A and B classification

Based on the scope of target analytes covered by the laboratories in this exercise, laboratories are subdi-vided into Categories (A and B) in accordance with the rules in the General Protocol (Appendix 8). To be classified into Category A a laboratory should

a) have analysed at least 90 % of the compulsory pesticides on the Target Pesticides List,b) have correctly reported concentration values for at least 90 % of the compulsory pesticides pre-

sent in the test item, c) not have reported any false positive results.

2. EVALUATION RULES / Laboratory Classification

13

Eva

luat

ion

Ru

lE

2

2.5.2 Combined z-Scores

For informative purposes and to allow comparison of the overall performance of the laboratories the Av-erage of the Absolute z-Scores (AAZ) is calculated for laboratories with 5 or more z-scores. Combined z-scores are, however, considered to be of lesser importance than the individual z-scores.

Average of the Absolute z-Scores (AAZ)

The AAZ is calculated using the following formula:

where “n” is the number of each laboratory’s z-scores that are considered in this formula. This includes z-scores assigned for false negative results. For the calculation, any z-score > 5 is set at 5.

AAZn

nz

AAZ ii∑

== 1

3. Participation

15

Part

iciP

atio

n

3

3. PARTICIPATION

121 laboratories from 37 countries (28 EU-Member States, 2 EFTA- countries, 1 EU-candidate country and 6 third countries) originally registered for participation in the EUPT-SRM13. An overview of the participating laboratories and countries is given in Table 3-1. A list of all individual laboratories that registered for this EUPT is presented in Appendix 1. Croatia was the only EU-country not represented by an NRL-SRM. Malta was represented by its proxy-NRL-SRM based in the United Kingdom.

Out of the 109 EU OfLs having registered for participation in the current PT five laboratories from Three co-nutries, among them the NRL-SRM in Italy, failed to submit any results and reported after the PT “technical problems/problems with instruments” or “target pesticides out of routien analytical scope” as the reason for no results submitted.

All 12 laboratories from non-EU countries submitted results (4 from EFTA countries, 2 from one EU-can-didate country and 6 from third countries). For the first time one OfL from Iceland has participated in an EUPT-SRM. The results submitted by the laboratories located in Serbia (EU candidate country) and by the 6 laboratories located in third countries were not taken into account when calculating the assigned values.

In total, 151 EU-OfLs, including NRL-SRMs, regardless of their commodity scope, as well as all EU-OfLs ana-lysing for pesticide residues in food and feed with high oil content and very low water content, were origi-nally considered as being obliged to participate in the present EUPT. These laboratories were invited to log in the registration page and register for their participation in the current PT or to provide an explanation for their non-participation.

30 obliged laboratories explained their non-participation with the fact that the matrix (soybeans) or the SRM13 target pesticides or both were out of their routine scope, partly due to a lack of required instru-ments. One obliged laboratory was not able to participate in because of the relocation of this laboratory. Excluding those 31 laboratories that provided sufficient explanations, the number of EU-laboratories con-sidered as being obliged decreased to 120. Out of the 92 obliged laboratories that have registered for this PT 88 laboratories finally submitted result. In addition, 17 OfLs registered for participation on voluntary basis, and 16 of them submitted results. Out of the 120 obliged OfLs 28 (23 %) did neither register for the PT nor provide any explanation for non-participation. These laboratories originated from 8 countries as fol-lows: HR (1×), FR (2×), DE (3×), IT (8×), PL (4×), RO (4×), ES (5×), and UK (1×).

In order to have sufficient results for evaluation of phosphine, eleven private laboratories worldwide were exceptionally invided to participate in the present PT. These private laboratories were also allowed to re-port results for any other pesticides in the target pesticides list if they wish. Participants from private labo-ratories will receive the certificate and the final report, however, their results, except those for phosphine, were not considered in the establishment of assigned values and their participation will not be shown in the final report.


16

EU: NRLs and OfLs

Contracting Country 1)

Labs originally

considered as obliged (*based on

scope)

Labs providing sufficient expl.

for non-participation Finally considered as obliged

Registered for Participation

Submitted Results Obliged labs

non particip. w/o

giving expl.

Notes

During Registration All NRL- SRMs All NRL-

SRMs

AL/ BE/ NL 1 1 1 1

AT 1 1 1 1 1 1

BE 6 1 5 5 + [1] 1 5 + [1] 1

BE/ BG/ FR/ LU 1 1 1 1

BG 2 1 1 1 1 1 1

CY 2 1 1 1 1 1 1 HR has not yet established an NRL-SRM.

CZ 3 3 3 1 3 1

DE 25 5 20 17 + [3] 1 16 + [3] 1 3

DE/ MT 1 1 1 1

DK 2 1 1 1 1 1 1

EE 3 1 2 2 1 2 1

FI 2 2 2 2 2 2 FI has appointed two NRL-SRMs.

FR 7 7 5 + [3] 1 5 + [3] 1 2

GR 2 2 2 + [1] 2 2 + [1] 2

HR 5 1 4 3 3 1 GR has appointed two NRL-SRMs.

HU 4 4 4 + [1] 1 4 + [1] 1

IE 1 1 1 1 1 1

IT 23 5 18 10 1 9 0 8

IT/ MT 1 1 1 1

LT 1 1 1 + [1] 1 1 + [1] 1

LU 1 1 1 1 1 1 *MT-NRL-SRM represented by proxy by the UK-NRL-SRM; MT subcontracted routine analy-sis to an OfLs in DE and IT

LV 1 1 1 1 1 1

MT 0* 0* 0* 0* 0* *MT-NRL-SRM represented by proxy by the UK-NRL-SRM; MT subcontracted routine analy-sis to an OfLs in DE and IT

NL 2 2 2 1 2 1

PL 11 5 6 2 + [1] 1 2 + [1] 1 4

PO 1 1 1 + [1] 1 + [1]

PT 1 1 1 1 1 1

RO 7 2 5 1 1 4

SE 2 2 2 1 2 1

SI 3 1 2 2 1 2 1

SK 1 1 1 1 1 1

ES 24 7 17 12 + [4] 2 10 + [3] 2 5 ES has appointed two NRL-SRMs

ES/ MT 1 1 1 1

UK/MT 1 1 1 1 1 1 UK-NRL-SRM represents also MT

UK 2 2 1 + [1] 1 + [1] 1

EU-total 151 31 120 92 + [17] 28 88 + [16] 27 28

Table 3-1: Number of laboratories listed as being obliged to participate in the EUPT-SRM13, labs that registered to participate, and labs that finally submitted results (grouped by contracting country)

3. Participation

17

Part

iciP

atio

n

3

Table 3-1 (cont.): Number of laboratories listed as being obliged to participate in the EUPT-SRM13, labs that registered to partici-pate, and labs that finally submitted results (grouped by contracting country)

EFTA

Contracting Country 1)

Labs originally

considered as obliged (*based on

scope)

Labs providing sufficient expl.

for non-participation Finally considered as

obliged

Registered for Participation

Submitted Results Obliged labs

non particip. w/o

giving expl.

NotesPrior to

PTDuring the

PT All NRL- SRMs All NRL-

SRMs

NO [1] 1 [1] 1

CH [3] – [3] –

EU+EFTA Total 92 + [21] 28 88 + [20] 27

Third Countries / EU candidate country

BR 1 – 1 –

BY 1 – 1 –

CR 1 – 1 –

PE 1 – 1 –

RS 2 – 2 –

SG 1 – 1 –

TH 1 – 1 –

Third Countries / EU candidate country Total 8 8

Overall Sum 120 121 28 116 27

4. RESULTS / Overview of Results

19

Resu

lts

4

4. RESULTS

4.1 Overview of Results

An overview of the percentage of laboratories having targeted each of the analytes present in the Target Pesticides List is shown in Table 4-1.

Table 4-2 (p. 20) gives an overview of all results submitted by each laboratory. The individual numerical results reported by the laboratories are shown in Table 4-8 (p. 36) and Table 4-9 (p. 42) for compulsory and optional, respectively. Detailed information about the analytical methods used by the laboratories is shown on the web under “EUPT-SRM13 - Supplementary Information” accessible via the the link: http://www.eurl-pesticides.eu/library/docs/srm/EUPT-SRM13_Supplementary_Information.pdf.

Labs analysed for the compound

CompoundsPresent

in test item

EU 1)- and EFTA-Labs EU obliged Labs only

No. 2) % (based on n = 109 3)) No. 2) % (based on n = 120 4))

Com

puls

ory

Com

poun

ds

2,4-D No 88 81 % 73 61 %

Bromide ion Yes 62 57 % 47 39 %

Chlormequat-Cl No 88 81 % 72 60 %

Cyromazine Yes 79 72 % 63 53 %

Ethephon No 75 69 % 60 50 %

Fluazifop Yes 86 79 % 70 58 %

Glyphosate Yes 83 76 % 68 57 %

Haloxyfop Yes 81 74 % 67 56 %

Mepiquat-Cl Yes 86 79 % 71 59 %

Opt

iona

l Com

poun

ds

2,4-DB Yes 52 48 % 43 36 %

Bentazone No 73 67 % 60 50 %

Carbofuran No 77 71 % 62 52 %

Chlorate No 56 51 % 42 35 %

Diquat Yes 30 28 % 21 18 %

Fenoxaprop No 41 38 % 33 28 %

Glufosinate Yes 44 40 % 33 28 %

MPP Yes 25 23 % 17 14 %

N-Acetyl-Glufosinate No 23 21 % 17 14 %

AMPA No 56 51 % 43 36 %

N-Acetyl-Glyphosate Yes 23 21 % 18 15 %

Paraquat No 29 27 % 21 18 %

Perchlorate Yes 55 50 % 41 34 %

Phosphonic acid Yes 45 41 % 32 27 %

Quizalofop Yes 62 57 % 50 42 %

Phsophine (Test Item) Yes 11 10 % 5 4 %

Phosphine (PH3-Tube) Yes 11 10 % 5 4 %

1) Including official laboratories participating on voluntary basis2) Laboratories representing more than one country were counted only once.3) 109 is the number of participating OfLs from EU and EFTA countries (including NRLs and official laboratories participating on voluntary basis)

having registered for the present PT and submitted at least one result.4) 120 is the number of OfLs (including NRLs) from EU countries, which were finally considered as obliged to participate in the EUPT-SRM13 (taking

into account any explanations for non-participation).

Table 4-1: Percentage of EU and EFTA laboratories that have analysed for the compounds in the Target Pesticides List

http://www.eurl-pesticides.eu/library/docs/srm/EUPT-SRM12_Supplementary_Information.pdf




20

Compulsory Compounds Optional Compounds Optional Compounds Total

Compulsory Compound listed in Target List 2,

4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

e

Carb

ofur

an

Chlo

rate Optional / Additional

Compound listed in Target List D

iqua

t

Feno

xapr

op

Glu

fosi

nate

MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

)

Phos

phin

e (P

H3-

Tube

)

Ana

lyse

d / c

orre

ctly

foun

d am

ong

OP

TIO

NA

L co

mpo

unds

(m

ax. 2

1 / 1

5)A

naly

sed

/ cor

rect

ly fo

und

amon

gCO

MPU

LSO

RY a

nd O

PTI

ON

AL

com

poun

ds

(max

. 21

/ 15)

within MACP 1) Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. Reg. WD – Reg. WD within MACP 1) WD – WD WD WD WD WD WD Cont. WD WD WD WD

present in Test Item No Yes No Yes No Yes Yes Yes Yes Yes No No No present in

Test Item Yes No Yes Yes No No Yes No Yes Yes Yes Yes Yes

evaluated in this PT No Yes No Yes No Yes Yes Yes Yes Yes No No No evaluated

in this PT Yes No Yes Yes No No Yes No Yes Yes Yes No No

Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

1 A ND V ND ND V V V V 8 / 5 V ND ND 1 A V ND ND ND 7 / 2 15 / 7

2 B ND V ND FN ND V V V FN 9 / 4 V ND ND ND 2 B V ND V ND ND FN V V 12 / 5 21 / 9

3 B ND V V V 4 / 3 V ND ND 3 B ND 4 / 1 8 / 4

4 x A ND V ND V ND V V V V 9 / 6 ND ND 4 x A V ND ND V V V V 9 / 5 18 / 11

5 x B ND ND ND V V V V 7 / 4 ND ND ND 5 x B V 4 / 1 11 / 5

6 A ND V ND V ND V V V V 9 / 6 ND ND ND 6 A V V V 6 / 3 15 / 9

7 x B ND V V V 4 / 3 V ND ND 7 x B ND 4 / 1 8 / 4

8 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 8 x A V V 6 / 3 15 / 9

10 A ND V ND V ND V V V V 9 / 6 ND ND ND 10 A ND V V V 7 / 3 16 / 9

11 A ND V ND V ND V V V V 9 / 6 V ND ND 11 A ND ND V FN FN V V 10 / 4 19 / 10

12 x A ND V ND V ND V V V V 9 / 6 V ND ND 12 x A ND ND V 6 / 2 15 / 8

13 x A ND V ND V ND V V V V 9 / 6 V ND ND 13 x A V ND V V ND ND V V V V 13 / 8 22 / 14

14 A ND V ND V ND V V V V 9 / 6 V ND ND ND 14 A V ND V ND ND V V V V V 14 / 8 23 / 14

15 A ND V ND V ND V V V V 9 / 6 ND ND ND 15 A V V ND ND V V V V 11 / 6 20 / 12

16 A ND V ND V ND V V V V 9 / 6 V ND ND ND 16 A ND V ND V V V V V 12 / 7 21 / 13

17 B ND ND V ND V V V 7 / 4 ND ND 17 B V ND V V V V V 9 / 6 16 / 10

19 x A ND V ND V ND V V V V 9 / 6 V ND ND 19 x A ND 4 / 1 13 / 7

20 x A ND V ND V ND V V V V 9 / 6 V ND ND 20 x A V 4 / 2 13 / 8

21 A ND V ND ND V V V V 8 / 5 ND ND 21 A V ND ND V ND 7 / 2 15 / 7

22 x A ND V ND V ND V V V V 9 / 6 V ND ND 22 x A V ND 5 / 2 14 / 8

23 B ND ND V V V V 6 / 4 V ND 23 B ND ND 4 / 1 10 / 5

24 x A ND ND V ND V V V V 8 / 5 V ND ND 24 x A 3 / 1 11 / 6

25 B ND V ND V V V V 7 / 5 ND ND 25 B 2 / 0 9 / 5

26 A ND V ND V ND V V V V 9 / 6 V ND ND ND 26 A V V V V 8 / 5 17 / 11

27 A ND V ND V ND V V V V 9 / 6 ND ND ND 27 A V ND V V ND ND ND V V V 13 / 6 22 / 12

28 B ND V 2 / 1 28 B 0 / 0 2 / 1

29 x A ND V ND V ND V V V V 9 / 6 ND ND 29 x A 2 / 0 11 / 6

1) MACP = EU Multiannual Control Program; Reg.: MACP Regulation; WD: NCP Working Document SANCO/12745/2013, 21 –22 November 2017 rev. 9(1) Cont.: Contaminant

2) Category A/B classification (Cat A was assigned to laboratories that have analysed at least 8 out of the 9 compulsory compounds on the Target Pesticides List, correctly detected 5 or more out of the 6 compulsory compounds present in the test item and have not reported any false positive result, see Section 4.4.4, p. 48)

V = analysed for and submitted concentration Value > “MRRL” for a pesticide present in the test item; ND = analysed for and correctly reported as “Not Detected”; Empty cells: not analysed; FN = analysed for but falsely not detected (False Negative result); FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as FN; FP = false positive result (FP): Result reported as “≤ MRRL” and, therefore, not regarded as FP.




Table 4-2: Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)


21

Resu

lts

4

Table 4-2 (cont.): Scope and categorization of participating laboratories (including third country laboratories and laboratories that have not submitted results)



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

e

Carb

ofur

an

Chlo



iqua

t

Feno

xapr

op

Glu

fosi

nate

MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

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tem

)

Phos

phin

e (P

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Tube

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Ana

lyse

d / c

orre

ctly

foun

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ong

OP

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NA

L co

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(m

ax. 2

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5)A

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/ cor

rect

ly fo

und

amon

gCO

MPU

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RY a

nd O

PTI

ON

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com

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ds

(max

. 21

/ 15)






Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

1 A ND V ND ND V V V V 8 / 5 V ND ND 1 A V ND ND ND 7 / 2 15 / 7

2 B ND V ND FN ND V V V FN 9 / 4 V ND ND ND 2 B V ND V ND ND FN V V 12 / 5 21 / 9

3 B ND V V V 4 / 3 V ND ND 3 B ND 4 / 1 8 / 4

4 x A ND V ND V ND V V V V 9 / 6 ND ND 4 x A V ND ND V V V V 9 / 5 18 / 11

5 x B ND ND ND V V V V 7 / 4 ND ND ND 5 x B V 4 / 1 11 / 5

6 A ND V ND V ND V V V V 9 / 6 ND ND ND 6 A V V V 6 / 3 15 / 9

7 x B ND V V V 4 / 3 V ND ND 7 x B ND 4 / 1 8 / 4

8 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 8 x A V V 6 / 3 15 / 9

10 A ND V ND V ND V V V V 9 / 6 ND ND ND 10 A ND V V V 7 / 3 16 / 9

11 A ND V ND V ND V V V V 9 / 6 V ND ND 11 A ND ND V FN FN V V 10 / 4 19 / 10

12 x A ND V ND V ND V V V V 9 / 6 V ND ND 12 x A ND ND V 6 / 2 15 / 8

13 x A ND V ND V ND V V V V 9 / 6 V ND ND 13 x A V ND V V ND ND V V V V 13 / 8 22 / 14

14 A ND V ND V ND V V V V 9 / 6 V ND ND ND 14 A V ND V ND ND V V V V V 14 / 8 23 / 14

15 A ND V ND V ND V V V V 9 / 6 ND ND ND 15 A V V ND ND V V V V 11 / 6 20 / 12


17 B ND ND V ND V V V 7 / 4 ND ND 17 B V ND V V V V V 9 / 6 16 / 10

19 x A ND V ND V ND V V V V 9 / 6 V ND ND 19 x A ND 4 / 1 13 / 7

20 x A ND V ND V ND V V V V 9 / 6 V ND ND 20 x A V 4 / 2 13 / 8

21 A ND V ND ND V V V V 8 / 5 ND ND 21 A V ND ND V ND 7 / 2 15 / 7

22 x A ND V ND V ND V V V V 9 / 6 V ND ND 22 x A V ND 5 / 2 14 / 8

23 B ND ND V V V V 6 / 4 V ND 23 B ND ND 4 / 1 10 / 5

24 x A ND ND V ND V V V V 8 / 5 V ND ND 24 x A 3 / 1 11 / 6

25 B ND V ND V V V V 7 / 5 ND ND 25 B 2 / 0 9 / 5

26 A ND V ND V ND V V V V 9 / 6 V ND ND ND 26 A V V V V 8 / 5 17 / 11

27 A ND V ND V ND V V V V 9 / 6 ND ND ND 27 A V ND V V ND ND ND V V V 13 / 6 22 / 12

28 B ND V 2 / 1 28 B 0 / 0 2 / 1

29 x A ND V ND V ND V V V V 9 / 6 ND ND 29 x A 2 / 0 11 / 6








22



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

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op

Mep

iqua

t-Cl

Ana

lyse

d / c

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ctly

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d am

ong

COM

PULS

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com

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ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

e

Carb

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Chlo



iqua

t

Feno

xapr

op

Glu

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MPP

N-A

cety

l-G

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te

AM

PA

N-A

cety

l-G

lyph

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Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

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Phso

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)

Phos

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Ana

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d / c

orre

ctly

foun

d am

ong

OP

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NA

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(m

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Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

30 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 30 x A V ND V V ND ND V ND V V V 15 / 8 24 / 14

31 A ND V ND V ND V V V V 9 / 6 ND ND ND 31 A V ND ND ND V V V 10 / 4 19 / 10

32 x A ND ND V ND V V V V 8 / 5 V ND ND ND 32 x A V ND ND ND V V V V V 13 / 7 21 / 12

33 A ND V ND V ND V V V V 9 / 6 V ND ND ND 33 A ND V ND V V V 10 / 5 19 / 11

34 A ND V ND V ND V V V V 9 / 6 V ND ND ND 34 A V ND V V ND ND V ND V V V V V 17 / 10 26 / 16

35 A ND ND V ND V V V V 8 / 5 V ND ND ND 35 A V V V ND ND V V V 12 / 7 20 / 12

36 x A ND ND V ND V V V V 8 / 5 V ND ND ND 36 x A V V V ND V ND V V V 13 / 8 21 / 13

37 A ND V ND V ND V V V V 9 / 6 ND 37 A V V ND ND V V V 8 / 5 17 / 11

38 B ND ND ND V V 5 / 2 ND 38 B ND V 3 / 1 8 / 3

39 B V 1 / 1 39 B 0 / 0 1 / 1

40 B V 1 / 1 40 B ND 1 / 0 2 / 1

41 B ND FP V V V 5 / 3 V 41 B V V ND FP V V V 8 / 6 13 / 9

42 B ND ND V V V V 6 / 4 ND 42 B ND 2 / 0 8 / 4

43 B V 1 / 1 43 B ND 1 / 0 2 / 1

44 B ND V 2 / 1 ND ND ND 44 B V ND V 6 / 2 8 / 3

45 B ND V ND V ND V V V V 9 / 6 V ND ND ND 45 B V ND V V FP ND FN ND V V V 15 / 7 24 / 13

46 A ND V ND V ND V V V V 9 / 6 V ND ND ND 46 A V ND V V ND ND V ND V V V 15 / 8 24 / 14

47 B 0 / 0 ND 47 B 1 / 0 1 / 0

48 A ND V ND V ND V V V V 9 / 6 ND ND ND 48 A ND ND V V V 8 / 3 17 / 9

49 x A ND V ND V ND V V V V 9 / 6 V ND 49 x A 2 / 1 11 / 7

50 A ND V ND V ND V V V V 9 / 6 V ND ND ND 50 A ND V V V 8 / 4 17 / 10

51 x B ND V ND V ND V V 7 / 4 51 x B 0 / 0 7 / 4

52 A ND V ND V ND V V V V 9 / 6 V ND ND ND 52 A V V V ND ND ND V V V 13 / 7 22 / 13

53 B ND ND V ND V V 6 / 3 ND 53 B 1 / 0 7 / 3

54 x A ND V ND V ND V V V V 9 / 6 ND ND 54 x A ND ND 4 / 0 13 / 6

55 A ND V ND V ND V V V V 9 / 6 FN ND ND 55 A FN ND FN V V 8 / 2 17 / 8

56 A ND V ND V ND V V V V 9 / 6 ND ND ND 56 A V 4 / 1 13 / 7









23

Resu

lts

4



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

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Carb

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Chlo



iqua

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Feno

xapr

op

Glu

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MPP

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cety

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AM

PA

N-A

cety

l-G

lyph

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Para

quat

Perc

hlor

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Phos

phon

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cid

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Phso

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tem

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Phos

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Ana

lyse

d / c

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ctly

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d am

ong

OP

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L co

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Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

30 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 30 x A V ND V V ND ND V ND V V V 15 / 8 24 / 14

31 A ND V ND V ND V V V V 9 / 6 ND ND ND 31 A V ND ND ND V V V 10 / 4 19 / 10

32 x A ND ND V ND V V V V 8 / 5 V ND ND ND 32 x A V ND ND ND V V V V V 13 / 7 21 / 12

33 A ND V ND V ND V V V V 9 / 6 V ND ND ND 33 A ND V ND V V V 10 / 5 19 / 11


35 A ND ND V ND V V V V 8 / 5 V ND ND ND 35 A V V V ND ND V V V 12 / 7 20 / 12

36 x A ND ND V ND V V V V 8 / 5 V ND ND ND 36 x A V V V ND V ND V V V 13 / 8 21 / 13

37 A ND V ND V ND V V V V 9 / 6 ND 37 A V V ND ND V V V 8 / 5 17 / 11

38 B ND ND ND V V 5 / 2 ND 38 B ND V 3 / 1 8 / 3

39 B V 1 / 1 39 B 0 / 0 1 / 1

40 B V 1 / 1 40 B ND 1 / 0 2 / 1

41 B ND FP V V V 5 / 3 V 41 B V V ND FP V V V 8 / 6 13 / 9

42 B ND ND V V V V 6 / 4 ND 42 B ND 2 / 0 8 / 4

43 B V 1 / 1 43 B ND 1 / 0 2 / 1

44 B ND V 2 / 1 ND ND ND 44 B V ND V 6 / 2 8 / 3

45 B ND V ND V ND V V V V 9 / 6 V ND ND ND 45 B V ND V V FP ND FN ND V V V 15 / 7 24 / 13


47 B 0 / 0 ND 47 B 1 / 0 1 / 0

48 A ND V ND V ND V V V V 9 / 6 ND ND ND 48 A ND ND V V V 8 / 3 17 / 9

49 x A ND V ND V ND V V V V 9 / 6 V ND 49 x A 2 / 1 11 / 7


51 x B ND V ND V ND V V 7 / 4 51 x B 0 / 0 7 / 4

52 A ND V ND V ND V V V V 9 / 6 V ND ND ND 52 A V V V ND ND ND V V V 13 / 7 22 / 13

53 B ND ND V ND V V 6 / 3 ND 53 B 1 / 0 7 / 3

54 x A ND V ND V ND V V V V 9 / 6 ND ND 54 x A ND ND 4 / 0 13 / 6

55 A ND V ND V ND V V V V 9 / 6 FN ND ND 55 A FN ND FN V V 8 / 2 17 / 8

56 A ND V ND V ND V V V V 9 / 6 ND ND ND 56 A V 4 / 1 13 / 7









24



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

e

Carb

ofur

an

Chlo



iqua

t

Feno

xapr

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Glu

fosi

nate

MPP

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cety

l-G

lufo

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AM

PA

N-A

cety

l-G

lyph

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e

Para

quat

Perc

hlor

ate

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phon

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cid

Qui

zalo

fop

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phin

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tem

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Phos

phin

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Ana

lyse

d / c

orre

ctly

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ong

OP

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Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

57 x B ND V V 3 / 2 ND ND 57 x B V 3 / 1 6 / 3

58 B V 1 / 1 58 B ND 1 / 0 2 / 1

59 B 0 / 0 59 B ND 1 / 0 1 / 0

60 A ND ND V ND V V V V 8 / 5 V ND ND 60 A ND V V ND ND V 9 / 4 17 / 9

61 x A ND ND V ND V V V V 8 / 5 ND ND 61 x A 2 / 0 10 / 5

62 B ND V ND V ND V V 7 / 4 ND ND 62 B V V ND ND V V V 9 / 5 16 / 9


64 B ND V 2 / 1 ND 64 B ND 2 / 0 4 / 1

65 A ND FN ND V V V V V 8 / 5 ND ND 65 A 2 / 0 10 / 5

66 B ND ND V V FN 5 / 2 ND ND 66 B 2 / 0 7 / 2

67 B ND V ND V V V V 7 / 5 ND ND ND 67 B V V ND V V V 9 / 5 16 / 10

68 x A ND V ND V ND V V V 8 / 5 ND ND 68 x A 2 / 0 10 / 5


70 B ND V V 3 / 2 70 B 0 / 0 3 / 2

71 A ND ND V ND V V V V 8 / 5 V ND ND ND 71 A V V ND ND V ND V 11 / 5 19 / 10


73 A ND ND V ND V V V V 8 / 5 ND ND 73 A V ND 4 / 1 12 / 6

74 x A ND V ND V ND V V V V 9 / 6 V ND ND 74 x A 3 / 1 12 / 7

76 x A ND ND V ND V V V V 8 / 5 V ND 76 x A V ND V ND ND FN ND 9 / 3 17 / 8

77 x B ND V V 3 / 2 ND 77 x B 1 / 0 4 / 2

78 x A ND V ND V ND V V V V 9 / 6 78 x A V 1 / 1 10 / 7

79 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 79 x A V V V 7 / 4 16 / 10

80 x B ND ND V V V V 6 / 4 ND 80 x B ND 2 / 0 8 / 4

82 B ND V V 3 / 2 ND ND 82 B 2 / 0 5 / 2


84 B ND V V V 4 / 3 ND 84 B 1 / 0 5 / 3

85 A ND V ND V ND V V V 8 / 5 V ND ND ND 85 A V FN FN 7 / 2 15 / 7









25

Resu

lts

4



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

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Carb

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an

Chlo



iqua

t

Feno

xapr

op

Glu

fosi

nate

MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

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Phos

phin

e (P

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Ana

lyse

d / c

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Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

57 x B ND V V 3 / 2 ND ND 57 x B V 3 / 1 6 / 3

58 B V 1 / 1 58 B ND 1 / 0 2 / 1

59 B 0 / 0 59 B ND 1 / 0 1 / 0

60 A ND ND V ND V V V V 8 / 5 V ND ND 60 A ND V V ND ND V 9 / 4 17 / 9

61 x A ND ND V ND V V V V 8 / 5 ND ND 61 x A 2 / 0 10 / 5

62 B ND V ND V ND V V 7 / 4 ND ND 62 B V V ND ND V V V 9 / 5 16 / 9


64 B ND V 2 / 1 ND 64 B ND 2 / 0 4 / 1

65 A ND FN ND V V V V V 8 / 5 ND ND 65 A 2 / 0 10 / 5

66 B ND ND V V FN 5 / 2 ND ND 66 B 2 / 0 7 / 2

67 B ND V ND V V V V 7 / 5 ND ND ND 67 B V V ND V V V 9 / 5 16 / 10

68 x A ND V ND V ND V V V 8 / 5 ND ND 68 x A 2 / 0 10 / 5


70 B ND V V 3 / 2 70 B 0 / 0 3 / 2

71 A ND ND V ND V V V V 8 / 5 V ND ND ND 71 A V V ND ND V ND V 11 / 5 19 / 10


73 A ND ND V ND V V V V 8 / 5 ND ND 73 A V ND 4 / 1 12 / 6

74 x A ND V ND V ND V V V V 9 / 6 V ND ND 74 x A 3 / 1 12 / 7

76 x A ND ND V ND V V V V 8 / 5 V ND 76 x A V ND V ND ND FN ND 9 / 3 17 / 8

77 x B ND V V 3 / 2 ND 77 x B 1 / 0 4 / 2

78 x A ND V ND V ND V V V V 9 / 6 78 x A V 1 / 1 10 / 7

79 x A ND V ND V ND V V V V 9 / 6 V ND ND ND 79 x A V V V 7 / 4 16 / 10

80 x B ND ND V V V V 6 / 4 ND 80 x B ND 2 / 0 8 / 4

82 B ND V V 3 / 2 ND ND 82 B 2 / 0 5 / 2


84 B ND V V V 4 / 3 ND 84 B 1 / 0 5 / 3

85 A ND V ND V ND V V V 8 / 5 V ND ND ND 85 A V FN FN 7 / 2 15 / 7









26



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

Gly

phos

ate

Hal

oxyf

op

Mep

iqua

t-Cl

Ana

lyse

d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

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Carb

ofur

an

Chlo



iqua

t

Feno

xapr

op

Glu

fosi

nate

MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

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Phos

phin

e (P

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Ana

lyse

d / c

orre

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foun

d am

ong

OP

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Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

86 A ND ND V ND V V V V 8 / 5 V ND ND ND 86 A V V ND V ND V V 11 / 6 19 / 11

87 A ND ND V ND V V V V 8 / 5 V ND ND ND 87 A V 5 / 2 13 / 7

88 A ND V ND V ND V V V V 9 / 6 V ND ND ND 88 A ND V V V V V 10 / 6 19 / 12

89 A ND V ND V ND V V V V 9 / 6 V ND ND ND 89 A V ND FN V ND ND FN ND V V V 15 / 6 24 / 12

90 B FN 1 / 0 ND 90 B 1 / 0 2 / 0

91 A ND V ND V ND V V V V 9 / 6 V ND ND ND 91 A ND V ND V V V V 11 / 6 20 / 12

92 A ND V ND V ND V V V V 9 / 6 ND 92 A V V V ND ND V 7 / 4 16 / 10

93 A ND V ND V ND V V V V 9 / 6 V ND ND ND 93 A V ND V ND ND V V V 12 / 6 21 / 12

94 B V 1 / 1 94 B 0 / 0 1 / 1

95 B V 1 / 1 95 B 0 / 0 1 / 1

96 B ND ND V V V V V 7 / 5 ND 96 B 1 / 0 8 / 5

97 A ND V ND V ND V V V V 9 / 6 V ND ND ND 97 A V ND V V ND ND V FN FN 13 / 5 22 / 11


99 B ND V 2 / 1 ND 99 B 1 / 0 3 / 1

100 x B ND V V V 4 / 3 100 x B 0 / 0 4 / 3

101 A ND ND V ND V V V V 8 / 5 V ND ND ND 101 A V ND V V ND ND ND V V V 14 / 7 22 / 12

102 B V 1 / 1 102 B 0 / 0 1 / 1

103 B V 1 / 1 103 B 0 / 0 1 / 1

104 A ND V ND V ND V V V V 9 / 6 104 A 0 / 0 9 / 6

105 A ND V ND V ND V V V V 9 / 6 V ND ND ND 105 A ND FN V ND ND V V V V 13 / 6 22 / 12

106 B ND V ND V V 5 / 3 106 B ND V V 3 / 2 8 / 5

107 B ND ND V V V V 6 / 4 V ND ND 107 B V V ND ND 7 / 3 13 / 7

109 A ND ND V ND V V V V 8 / 5 FN ND ND ND 109 A FN V FN ND ND FN ND FN 12 / 1 20 / 6

110 B ND ND V V 4 / 2 ND 110 B V ND ND V 5 / 2 9 / 4

111 B V ND ND V 4 / 2 ND 111 B V 2 / 1 6 / 3









27

Resu

lts

4



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

zifo

p

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ate

Hal

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op

Mep

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d / c

orre

ctly

foun

d am

ong

COM

PULS

ORY

com

poun

ds

(max

. 13

/ 8)

2,4-

DB

Bent

azon

e

Carb

ofur

an

Chlo



iqua

t

Feno

xapr

op

Glu

fosi

nate

MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

)

Phos

phin

e (P

H3-

Tube

)

Ana

lyse

d / c

orre

ctly

foun

d am

ong

OP

TIO

NA

L co

mpo

unds

(m

ax. 2

1 / 1

5)A

naly

sed

/ cor

rect

ly fo

und

amon

gCO

MPU

LSO

RY a

nd O

PTI

ON

AL

com

poun

ds

(max

. 21

/ 15)






Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)

86 A ND ND V ND V V V V 8 / 5 V ND ND ND 86 A V V ND V ND V V 11 / 6 19 / 11

87 A ND ND V ND V V V V 8 / 5 V ND ND ND 87 A V 5 / 2 13 / 7

88 A ND V ND V ND V V V V 9 / 6 V ND ND ND 88 A ND V V V V V 10 / 6 19 / 12

89 A ND V ND V ND V V V V 9 / 6 V ND ND ND 89 A V ND FN V ND ND FN ND V V V 15 / 6 24 / 12

90 B FN 1 / 0 ND 90 B 1 / 0 2 / 0

91 A ND V ND V ND V V V V 9 / 6 V ND ND ND 91 A ND V ND V V V V 11 / 6 20 / 12

92 A ND V ND V ND V V V V 9 / 6 ND 92 A V V V ND ND V 7 / 4 16 / 10

93 A ND V ND V ND V V V V 9 / 6 V ND ND ND 93 A V ND V ND ND V V V 12 / 6 21 / 12

94 B V 1 / 1 94 B 0 / 0 1 / 1

95 B V 1 / 1 95 B 0 / 0 1 / 1

96 B ND ND V V V V V 7 / 5 ND 96 B 1 / 0 8 / 5

97 A ND V ND V ND V V V V 9 / 6 V ND ND ND 97 A V ND V V ND ND V FN FN 13 / 5 22 / 11


99 B ND V 2 / 1 ND 99 B 1 / 0 3 / 1

100 x B ND V V V 4 / 3 100 x B 0 / 0 4 / 3

101 A ND ND V ND V V V V 8 / 5 V ND ND ND 101 A V ND V V ND ND ND V V V 14 / 7 22 / 12

102 B V 1 / 1 102 B 0 / 0 1 / 1

103 B V 1 / 1 103 B 0 / 0 1 / 1

104 A ND V ND V ND V V V V 9 / 6 104 A 0 / 0 9 / 6

105 A ND V ND V ND V V V V 9 / 6 V ND ND ND 105 A ND FN V ND ND V V V V 13 / 6 22 / 12

106 B ND V ND V V 5 / 3 106 B ND V V 3 / 2 8 / 5

107 B ND ND V V V V 6 / 4 V ND ND 107 B V V ND ND 7 / 3 13 / 7

109 A ND ND V ND V V V V 8 / 5 FN ND ND ND 109 A FN V FN ND ND FN ND FN 12 / 1 20 / 6

110 B ND ND V V 4 / 2 ND 110 B V ND ND V 5 / 2 9 / 4

111 B V ND ND V 4 / 2 ND 111 B V 2 / 1 6 / 3









28



4-D

Brom

ide

ion

Chlo

rmeq

uat-

Cl

Cyro

maz

ine

Ethe

phon

Flua

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p

Gly

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Hal

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Ana

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ctly

foun

d am

ong

COM

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(max

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/ 8)

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Carb

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Chlo



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Feno

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Glu

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N-A

cety

l-G

lufo

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AM

PA

N-A

cety

l-G

lyph

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e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

)

Phos

phin

e (P

H3-

Tube

)

Ana

lyse

d / c

orre

ctly

foun

d am

ong

OP

TIO

NA

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unds

(m

ax. 2

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5)A

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rect

ly fo

und

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gCO

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RY a

nd O

PTI

ON

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com

poun

ds

(max

. 21

/ 15)






Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)


113 B 0 / 0 113 B V V 2 / 2 2 / 2

114 B 0 / 0 114 B V V 2 / 2 2 / 2

3rd-115 B ND ND V V FN V 6 / 3 FN ND 3rd-115 B V V ND 5 / 2 11 / 5

3rd-116 B ND V ND V ND V V V 8 / 5 ND ND 3rd-116 B V V 4 / 2 12 / 7

3rd-117 A ND V ND V ND V V V V 9 / 6 V ND 3rd-117 A V ND ND 5 / 2 14 / 8

3rd-118 B ND V V ND FN V 6 / 3 ND ND 3rd-118 B V ND FP FP 6 / 1 12 / 4

3rd-119 B ND V 2 / 1 V ND 3rd-119 B 2 / 1 4 / 2

3rd-120 B ND ND V 3 / 1 ND 3rd-120 B V ND 3 / 1 6 / 2

3rd-121 B ND V 1 / 1 ND ND 3rd-121 B FN* ND 1 / 0 2 / 1

3rd-122 B ND V V ND V V V 7 / 5 3rd-120 B V 1 / 1 8 / 6









29

Resu

lts

4




4-D

Brom

ide

ion

Chlo

rmeq

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Cl

Cyro

maz

ine

Ethe

phon

Flua

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p

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Hal

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Feno

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Glu

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MPP

N-A

cety

l-G

lufo

sina

te

AM

PA

N-A

cety

l-G

lyph

osat

e

Para

quat

Perc

hlor

ate

Phos

phon

ic a

cid

Qui

zalo

fop

Phso

phin

e (T

est I

tem

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Phos

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H3-

Tube

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Ana

lyse

d / c

orre

ctly

foun

d am

ong

OP

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NA

L co

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unds

(m

ax. 2

1 / 1

5)A

naly

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rect

ly fo

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gCO

MPU

LSO

RY a

nd O

PTI

ON

AL

com

poun

ds

(max

. 21

/ 15)






Lab- Code SRM13-

NRL- SRM Cat. 2)

Lab- Code SRM13-

NRL- SRM Cat. 2)


113 B 0 / 0 113 B V V 2 / 2 2 / 2

114 B 0 / 0 114 B V V 2 / 2 2 / 2

3rd-115 B ND ND V V FN V 6 / 3 FN ND 3rd-115 B V V ND 5 / 2 11 / 5

3rd-116 B ND V ND V ND V V V 8 / 5 ND ND 3rd-116 B V V 4 / 2 12 / 7

3rd-117 A ND V ND V ND V V V V 9 / 6 V ND 3rd-117 A V ND ND 5 / 2 14 / 8

3rd-118 B ND V V ND FN V 6 / 3 ND ND 3rd-118 B V ND FP FP 6 / 1 12 / 4

3rd-119 B ND V 2 / 1 V ND 3rd-119 B 2 / 1 4 / 2

3rd-120 B ND ND V 3 / 1 ND 3rd-120 B V ND 3 / 1 6 / 2

3rd-121 B ND V 1 / 1 ND ND 3rd-121 B FN* ND 1 / 0 2 / 1

3rd-122 B ND V V ND V V V 7 / 5 3rd-120 B V 1 / 1 8 / 6








30

Table 4-3: Numerical values of analyte concentration in the blank material reported by the participating laboratories

Compound MRRL

[mg/kg]Assigned Value

[mg/kg]

Conc. in Blank Material

[mg/kg]

Conc. in Test Item

[mg/kg]

RL

[mg/kg] Reported by

Bromide ion 2 15.4 0.14 4.29 1 SRM13-74

0.374 9.886 0.05 SRM13-34

0.4 14.1 2 SRM13-72

0.543 14.4 0.3 SRM13-3rd-118

0.66 15.9 0.2 SRM13-45

0.702 12.9 2 SRM13-92

0.725 14.1 2 SRM13-67

0.783 17.8 0.2 SRM13-13

0.8 14.6 0.5 SRM13-6

1.2 12 1 SRM13-112

1.5 11.6 1 SRM13-98

3.7 18 2 SRM13-31

10.4 27.9 5 SRM13-97

Glyphosate 0.03 0.903 0.002 0.859 0.01 SRM13-98

AMPA 0.05 not present 0.0923 0.0906 (= FP) 0.05 SRM13-3rd-118

Paraquat 0.02 not present 0.497 0.495 (= FP) 0.05 SRM13-3rd-118

Perchlorate 0.01 0.100 0.0035 0.0825 0.005 SRM13-67

0.004 0.102 0.01 SRM13-98

Phosphonic acid 0.05 1.87 0.02 1.59 0.01 SRM13-14

0.039 2.45 0.05 SRM13-98

Phsophine (Test Item) 0.005 – 0.00001 0.21 0.0001 SRM13-113

Phosphine (PH3-Tube) 0.005 – 0.00001 0.106 0.0001 SRM13-113

4.2 Analysis of Blank Material

In 68 cases the laboratories reported detecting of target pesticides in the blank material under their report-ing limit or MRRLs (data not shown). In further 22 cases (Table 4-3) the laboratories reported numerical re-sults for the concentration of taget pesticides detected in the blank material, among them there were four cases (2× bromide ion, 1× paraquat and 1× AMPA) where participants reported detections in the blank ma-terial at levels higher than both their own RLs and above the MRRL. All these four cases indicated contami-nation in the procedure or background value in the system. In the two cases of paraquat (MRRL = 0.02 mg/kg) at 0.497 mg/kg and AMPA (MRRL = 0.05 mg/kg) at 0.0923 mg/kg, both reported by SRM13-3rd-118, this laboratory has also detected these two analytes in the test item at the comparable levels although they were neither spiked to the test item nor detected by other laboratories. In the two cases of bromide ion (MRRL = 2 mg/kg) at 3.7 mg/kg (reported by SRM13-31) and 10.4 mg/kg (reported by SRM13-97) the par-ticipants would have achieved much better z-scores if the reported results would have been substrated from the concentration in the blank material. The affected laboratories are encouraged to find the reasons behind these contamination / background value.

4.3 Assigned Values and Target Standard Deviations

The assigned value (xpt) of each analyte present in the test item was established as the mean of robust sta-tistics (x*) of all numerical results submitted by laboratories from EU and EFTA countries calculated using Algorithm A [6, Appendix 8]. Results from third country laboratories were not taken into account. Except the calculation of phosphine the results reported by private laboratories were also not taken into account. Based on these assigned values, z-scores were calculated for all submitted results using the FFP-approach

4. RESULTS / Assigned Values and Target Standard Deviations

31

Resu

lts

4

(Section 4.4.3, p. 34), and a preliminary report was released on 19 June, 2018. The uncertainties (u(xpt)) of the assigned values were calculated as described under Section 2.2, p. 11.

In the case of diquat the very wide distribution of participants’ results (CV* 52.8 %) resulted in the robust mean being assosiated with a statistical uncertainty exceeding the tolerance (Table 4-5, p. 32). The Sci-entific Committee therefore decided to evaluate the robust mean and z-scores for diquat for informative purposes only.

In the case of phosphine (both in the test item and in the PH3-tube), althouth the results submitted from private laboratories routinely analysing this compound were taken into account, the total number of re-sults (18) were low and the results distribution were extremely wide with a CV*-value of 93.1 % for phos-phine in the test item and 74.8 % for phosphine in the PH3-Tube. A reliable statistical evaluation for these two parameter was therefore not possible. A special report on phsophine with discussion about the ana-lytical difficulties will be issued.

The CV*-values of all other compulsory and optional analytes were lower than the FFP-RSD of 25 %. The av-erage CV*s of compulsory analytes based on the entire population of EU-and EFTA-laboratories was 21.2 %, and the average CV*s of optional analytes based on the entire population excluding diquat, phosphine (test tiem) and phosphine (PH-Tube) was 22.0 %. Both were clearly lower than the FFP-RSD of 25 %.

Table 4-4: Assigned values, uncertainties of assigned values and CV* values calculated for all compounds present in the test item

Assigned Value and CV* Based on the Entire Population of Results from EU and EFTA Laboratories

Compound No. of FNs

No. of numerical

results (EU+EFTA)

Assigned Value

[mg/kg]

u(xpt) 1) [mg/kg]

u(xpt) Tolerance

[mg/kg]

Judgementfor

UAV-testCV* 2)

[%]

Com

puls

ory

Co

mpo

unds

Bromide ion 1 61 15.3 +/-0.58988 1.1517 passed 24.0

Cyromazine 1 78 0.097 +/-0.00323 0.0073 passed 23.5

Fluazifop 1 85 0.049 +/-0.00136 0.0037 passed 20.3

Glyphosate 83 0.903 +/-0.02798 0.0677 passed 22.6

Haloxyfop 81 0.017 +/-0.00048 0.013 passed 20.4

Mepiquat-Cl 2 84 0.124 +/-0.00387 0.0093 passed 22.9

Average 3) CV* 21.2

Opt

iona

l Co

mpo

unds

2,4-DB 2 50 0.183 +/-0.00669 0.0137 passed 20.7

Diquat 4) 1 29 1.70 +/-0.20868 0.1267 failed 52.8 4)

Glufosinate 3 41 0.192 +/-0.01073 0.0144 passed 28.7

MPP 1 24 0.188 +/-0.00908 0.0141 passed 18.9

N-Acetyl-Glyphosate 5 18 0.835 +/-0.05185 0.0626 passed 21.1

Perchlorate 2 53 0.100 +/-0.00289 0.0075 passed 16.9

Phosphonic acid 3 42 1.86 +/-0.08723 0.1398 passed 24.3

Quizalofop 2 60 0.052 +/-0.00198 0.0039 passed 23.6

Phsophine (Test Item) 5) 11 + 7 6) 0.092 +/-0.02517 0.0069 failed 93.1 5)

Phosphine (PH3-Tube) 5) 11 + 7 6) 0.040 +/-0.00877 0.003 failed 74.8 5)

Average 3) CV* 22.0

1: u(xpt) : Uncertainty of assigned value calculated as shown under Section 2.2 (p. 38)2: CV* : Relative standard deviation based on robust statistics3: The average CV* is given for information purposes only. CV*s of individual compounds or average CV*s of individual compounds or related

compounds over many PTs are more meaningfull and conclusive.4: Excluded from the calculation of the average CV*s and the assigned values as well as z-scores were calculated for informative purpose only.5: Excluded from the calculation of the average CV*s and from this report, will be evaluated and discussed in a separate report.6: 7 results reported by private laboratories which were exceptionally invited to analyte phosphine


32

4.4 Assessment of Laboratory Performance

4.4.1 False Positives

Five results were preliminarily judged as false positives: AMPA (2x), ethephon (1x), N-acetyl glufosinate (1x) and paraquat (1x). In cases where the reported concentration of a compound not present in the Test Item was lower than the respective MRRL the results were preliminarily not judged as false positives. This con-cerned carbofuran, chlorate and AMPA in one case each.

Among EU- and EFTA-laboratories three laboratories reported in three cased numerical results for three analytes (ethephon, N-Acetyl-Glufosinate and AMPA) on the Target Pesticides List but not present in the test material. Two other false positive results (AMLA and paraquat) were reported by one laboratory from third countries. All these analytes were neither detected by the organisers nor by the overwhelming majority of the participants (Table 4-5). These five results exceeded the laboratories’ reporting limits for these com-pounds, were higher than the respective MRRLs in the Target Pesticides List, and were, therefore, judged as false positives.

Three laboratories reported in three cases numerical results for carbofuran (0.0028 mg/kg), chlorate (0.0043 mg/kg), and AMPA (0.002 mg/kg), which were lower than the laboratories’ RLs or MRRL. Following the rules in the General Protocol these two results were not judged as false positives, although they actu-ally should not be reported.

4.4.2 False Negatives

Among the compulsory compounds there were 7 cases (2× fluazifop, 2× Mepiquat-Cle-Cl, 1× bromide ion, 1× cyromazine and 1× haloxyfop) where the participants reported “analysed, but not detected” for target compounds which were spiked to the test item and detected by the majority of the laboratories target-ing them (Table 4-6, p. 33). Five of them were reported by laboratories from EU and EFTA countries and represented 1.0 % of the total 477 results reported by the EU/EFTA laboratories for compulsory target compounds present in the test item. The total 7 esults, including the other two reportet by laboratories from third countires, represented 1.4 % of the total 504 results from all participating laboratories. As the as-signed values for these seven analytes were sufficiently distant from the MRRLs, these results were judged as false negatives. In one case of cyromazine the “false negative” judgement resulted from the fact that the laboratory had a reporting limit at a similar level to the assigned value.

Compound PT-Code Analysed Reported Result [mg/kg]

RL [mg/kg]

MRRL [mg/kg] Judgement

Ethephon SRM13-41 Yes 0.368 0.01 0.02 FP

Opt

iona

l Com

poun

ds

Carbofuran SRM13-7 Yes 0.0028 – 0.005 –

Chlorate SRM13-67 Yes 0.0043 0.005 0.01 –

N-Acetyl-Glufosinate SRM13-45 Yes 1.26 0.02 0.02 FP

AMPA SRM13-41 Yes 0.078 0.01 0.05 FP

SRM13-98 Yes 0.002 0.01 0.05 –

SRM13-3rd-118 Yes 0.0906 0.05 0.05 FP

Paraquat SRM13-3rd-118 Yes 0.495 0.05 0.02 FP

Table 4-5: Overview of false positive and potentially false positive results reported by participating laboratories

4. RESULTS / Assessment of Laboratory Performance

33

Resu

lts

4

Compound PT-Code Analysed Detected RL [mg/kg]

MRRL [mg/kg]

Assigned Value

[mg/kg]Judgement

Com

puls

ory

Com

poun

ds

Bromide ion SRM13-65 Yes No 12.5 2 15.4 False Negative

Cyromazine SRM13-2 Yes No 0.01 0.01 0.097 False Negative

Fluazifop SRM13-90 Yes No 0.005 0.01 0.049 False Negative

SRM13-3rd-118 Yes No 0.01 False Negative

Haloxyfop SRM13-3rd-115 Yes No 0.003 0.003 0.017 False Negative

Mepiquat-Cl SRM13-2 Yes No 0.01 0.01 0.124 False Negative

SRM13-66 Yes No 0.01 False Negative

Opt

iona

l Com

poun

ds

2,4-DB SRM13-55 Yes No 0.01 0.01 0.183 False Negative



Diquat SRM13-109 Yes No 0.02 0.02 1.70 False Negative

Glufosinate SRM13-55 Yes No 0.04 0.02 0.192 False Negative



SRM13-3rd-121 Yes No 0.5 False Negative*

MPP SRM13-109 Yes No 0.02 0.02 0.188 False Negative

N-Acetyl- Glyphosate

SRM13-45 Yes No 0.02 0.02 0.835 False Negative


SRM13-76 Yes No mg/kg False Negative



Perchlorate SRM13-2 Yes No 0.01 0.01 0.100 False Negative


Phosphonic acid SRM13-11 Yes No 0.05 0.05 1.86 False Negative



Quizalofop SRM13-47 Yes No – 0.01 0.052 False Negative




*: Laboratory’s RL >> MRRL; in accordance with the General Protocole judged as false negative.

Table 4-6: Overview of false negative results reported by participating laboratories (including 3rd country laboratories)

Among the optional compounds there were 23 cases (4× N-acetyl-glyphosate, 4× Quizalofop, 3× 2,4-DB, 4× glufosinate, 3× phosphonic acid, 2× perchlorate, 1× diquat and 1× MPP) where the participants report-ed “analysed, but not detected” for target compounds that were spiked to the test item and detected by the majority of the laboratories targeting them (Table 4-6). In one case of glufosinate the “false negative” judgement resulted from the fact that the laboratory had a higher reporting limit than the assigned value, as this is the rule stated in the General Protocol. The 19 false negative results reported by EU/EFTA labora-tories accounted for 5.3 % of the total 358 results reported by the EU/EFTA laboratories for optional target compounds. The 23 false negative results reported in total represented 6.2 % of the 372 results reported by all participating labs for optional compounds.


34

4.4.3 Laboratory Performance Based on z-Scores

All individual z-scores were calculated using the FFP-RSD of 25 % and the assigned values derived from the entire population of results received from EU/EFTA laboratories. Table 4-7 shows the overall classification of z-scores achieved by all laboratories for compulsory and optional compounds. The respective rules are shown in Section 2.4 (p. 12). Among the laboratories from EU and EFTA countries “Acceptable” z-scores were achieved by 82 – 97 % (91 % on average) of the labs in the case of compulsory compounds and by 74 – 92 % (85 % on average) in the case of optional compounds excluding diquat and phosphine. Overall, 89 % of the results submitted by EU- and EFTA-countries were acceptable, 5 % questionable and 10 % unac-ceptable (including false negatives). The respective overall figures of 3rd country labs were 74 %, 5 % and 21 %.

A compilation of all individual results and z-scores for each laboratory is shown in Table 4-8 (p. 36) and Table 4-9 (p. 42) for compulsory and optional compounds, respectively. The corresponding kernel density histograms showing the distribution of the reported results are shown in Appendix 5. A graphic represen-tation of the z-score distribution of each target analyte present in the test item can be seen in Appendix 6.


35

Resu

lts

4

Table 4-7: Overall performance based on z-score classification

EU and EFTA laboratories

Compound No. of results 1)

Acceptable Questionable Unacceptable 1) FNs

No. (%) No. (%) No. (%) No.

Com

puls

ory

Com

poun

ds

Bromide ion 62 56 (90 %) 2 (3 %) 4 (6 %) 1

Cyromazine 79 65 (82 %) 8 (10 %) 6 (8 %) 1

Fluazifop 86 83 (97 %) 2 (2 %) 1 (1 %) 1

Glyphosate 83 78 (94 %) 2 (2 %) 3 (4 %) 0

Haloxyfop 81 78 (96 %) 2 (2 %) 1 (1 %) 0

Mepiquat-Cl 86 76 (88 %) 2 (2 %) 8 (9 %) 2

Subtotal (average) 477 436 (91 %) 18 (4 %) 23 (5 %) 5

Opt

iona

l Co

mpo

unds

2)

2,4-DB 52 48 (92 %) 1 (2 %) 3 (6 %) 2

Glufosinate 44 37 (84 %) 2 (5 %) 5 (11 %) 3

MPP 25 20 (80 %) 2 (8 %) 3 (12 %) 1

N-Acetyl-Glyphosate 23 17 (74 %) (0 %) 6 (26 %) 5

Perchlorate 55 47 (85 %) 3 (5 %) 5 (9 %) 2

Phosphonic acid 45 36 (80 %) 2 (4 %) 7 (16 %) 3

Quizalofop 62 54 (87 %) 5 (8 %) 3 (5 %) 2


Overall EU/EFTA (Average) 783 695 (89 %) 33 (4 %) 55 (7 %) 23

3rd country laboratories

Compound No. of results 1)

Acceptable Questionable Unacceptable 1) FNs

No. (%) No. (%) No. (%) No.

Com

puls

ory

Com

poun

ds

Bromide ion 4 4 (100 %) 0 (0 %) 0

Cyromazine 5 4 (80 %) 1 (20 %) 0 (0 %) 0

Fluazifop 3 2 (67 %) 1 (33 %) 1

Glyphosate 7 6 (86 %) 1 (14 %) 0

Haloxyfop 4 2 (50 %) 1 (25 %) 1 (25 %) 1

Mepiquat-Cl 4 3 (75 %) 1 (25 %) 0


Opt

iona

l Co

mpo

unds

2)

2,4-DB 3 2 (67 %) (0 %) 1 (33 %) 1

Glufosinate 6 5 (83 %) (0 %) 1 (17 %) 1

MPP

N-Acetyl-Glyphosate

Perchlorate

Phosphonic acid

Quizalofop 2 (0 %) (0 %) 2 (100 %) 2


Overall 3rd country (Average) 38 28 (74 %) 2 (5 %) 8 (21 %) 6

1) including false negatives (FNs)2) excluding diquat and phosphine


36

COMPULSORY Compound Bromide ion Cyromazine Fluazifop COMPULSORY Compound Glyphosate Haloxyfop Mepiquat-Cl

MRRL [mg/kg] 2 0.01 0.01 MRRL [mg/kg] 0.03 0.003 0.01

Assigned Value [mg/kg] 15.356 0.097 0.049 Assigned Value [mg/kg] 0.903 0.017 0.124

CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM

Analysed / corr. found, max. 13 / 8

Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

1 8 / 5 A 20.5 1.3 0.0534 0.3 1 8 / 5 A 0.922 0.1 0.0159 -0.2 0.123 0.0

2 9 / 4 B 15.5 0.0 FN -3.6 0.052 0.2 2 9 / 4 B 0.631 -1.2 0.014 -0.7 FN -3.7

3 4 / 3 B 0.0818 -0.6 0.0463 -0.2 3 4 / 3 B 0.0147 -0.5

4 x 9 / 6 A 18.5 0.8 0.1 0.1 0.0718 1.8 4 x 9 / 6 A 0.926 0.1 0.016 -0.2 0.124 0.0

5 x 7 / 4 B 0.0473 -0.2 5 x 7 / 4 B 0.4327 -2.1 0.0241 1.7 0.0829 -1.3

6 9 / 6 A 14.6 -0.2 0.107 0.4 0.0485 -0.1 6 9 / 6 A 0.95 0.2 0.0127 -1.0 0.115 -0.3

7 x 4 / 3 B 0.113 0.7 0.0335 -1.3 7 x 4 / 3 B 0.0157 -0.3

8 x 9 / 6 A 16.4 0.3 0.111 0.6 0.0466 -0.2 8 x 9 / 6 A 0.924 0.1 0.0151 -0.4 0.12 -0.1

10 9 / 6 A 14.8 -0.1 0.0464 -2.1 0.0213 -2.3 10 9 / 6 A 0.999 0.4 0.0151 -0.4 0.11 -0.4

11 9 / 6 A 14.3 -0.3 0.102 0.2 0.0539 0.4 11 9 / 6 A 1.12 1.0 0.0177 0.2 0.0959 -0.9

12 x 9 / 6 A 12.8 -0.7 0.1 0.1 0.052 0.2 12 x 9 / 6 A 1.04 0.6 0.017 0.0 0.154 1.0

13 x 9 / 6 A 17.8 0.6 0.23 5.5 0.038 -0.9 13 x 9 / 6 A 1.06 0.7 0.0139 -0.7 0.301 5.7

14 9 / 6 A 14.8 -0.1 0.112 0.6 0.0701 1.7 14 9 / 6 A 0.821 -0.4 0.0181 0.3 0.12 -0.1

15 9 / 6 A 12.1 -0.8 0.0997 0.1 0.0632 1.1 15 9 / 6 A 0.733 -0.8 0.0181 0.3 0.128 0.1

16 9 / 6 A 19.3 1.0 0.072 -1.0 0.062 1.0 16 9 / 6 A 1.17 1.2 0.019 0.5 0.131 0.2

17 7 / 4 B 0.0848 -0.5 0.0426 -0.5 17 7 / 4 B 0.615 -1.3 0.0182 0.3

19 x 9 / 6 A 20.3 1.3 1.18 44.7 0.068 1.5 19 x 9 / 6 A 1.22 1.4 0.017 0.0 1.33 39.0

20 x 9 / 6 A 16.5 0.3 0.101 0.2 0.0422 -0.6 20 x 9 / 6 A 0.969 0.3 0.0144 -0.6 0.149 0.8

21 8 / 5 A 14.3 -0.3 0.048 -0.1 21 8 / 5 A 0.839 -0.3 0.016 -0.2 0.147 0.7

22 x 9 / 6 A 16.4 0.3 0.0772 -0.8 0.0406 -0.7 22 x 9 / 6 A 1.05 0.7 0.0147 -0.5 0.132 0.3

23 6 / 4 B 0.052 0.2 23 6 / 4 B 1.02 0.5 0.017 0.0 0.138 0.5

24 x 8 / 5 A 0.121 1.0 0.065 1.3 24 x 8 / 5 A 1 0.4 0.021 1.0 0.167 1.4

25 7 / 5 B 18.7 0.9 0.118 0.9 0.052 0.2 25 7 / 5 B 0.019 0.5 0.125 0.0

26 9 / 6 A 15.0 -0.1 0.085 -0.5 0.032 -1.4 26 9 / 6 A 0.65 -1.1 0.011 -1.4 0.16 1.2

27 9 / 6 A 17.3 0.5 0.084 -0.5 0.046 -0.3 27 9 / 6 A 1.02 0.5 0.01 -1.6 0.15 0.8

28 2 / 1 B 0.0565 0.6 28 2 / 1 B

29 x 9 / 6 A 23.61 2.1 0.08 -0.7 0.072 1.8 29 x 9 / 6 A 0.893 0.0 0.015 -0.4 0.089 -1.1

30 x 9 / 6 A 12.9 -0.6 0.114 0.7 0.049 0.0 30 x 9 / 6 A 1.04 0.6 0.049 7.6 0.149 0.8

31 9 / 6 A 18.0 0.7 0.075 -0.9 0.049 0.0 31 9 / 6 A 0.959 0.2 0.016 -0.2 0.108 -0.5

32 x 8 / 5 A 0.0842 -0.5 0.0455 -0.3 32 x 8 / 5 A 1.02 0.5 0.0157 -0.3 0.118 -0.2

33 9 / 6 A 11.3 -1.1 0.092 -0.2 0.0531 0.3 33 9 / 6 A 0.883 -0.1 0.017 0.0 0.118 -0.2

34 9 / 6 A 9.886 -1.4 0.105 0.3 0.047 -0.2 34 9 / 6 A 0.779 -0.5 0.016 -0.2 0.088 -1.2

35 8 / 5 A 0.04 -2.3 0.037 -1.0 35 8 / 5 A 1.23 1.4 0.011 -1.4 0.151 0.9

36 x 8 / 5 A 0.0786 -0.8 0.0496 0.0 36 x 8 / 5 A 0.721 -0.8 0.0171 0.1 0.0841 -1.3

37 9 / 6 A 16.4 0.3 0.087 -0.4 0.057 0.6 37 9 / 6 A 1.29 1.7 0.022 1.2 0.15 0.8

38 5 / 2 B 0.0483 -0.1 38 5 / 2 B 0.131 0.2

39 1 / 1 B 39 1 / 1 B 0.983 0.4

40 1 / 1 B 40 1 / 1 B 1.09 0.8

41 5 / 3 B 0.0686 1.6 41 5 / 3 B 1.17 1.2 0.0226 1.4

42 6 / 4 B 0.075 -0.9 0.038 -0.9 42 6 / 4 B 0.014 -0.7 0.111 -0.4

43 1 / 1 B 43 1 / 1 B 0.794 -0.5

44 2 / 1 B 44 2 / 1 B 1.989 4.8

* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)


Table 4-8: Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds


37

Resu

lts

4




CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

1 8 / 5 A 20.5 1.3 0.0534 0.3 1 8 / 5 A 0.922 0.1 0.0159 -0.2 0.123 0.0

2 9 / 4 B 15.5 0.0 FN -3.6 0.052 0.2 2 9 / 4 B 0.631 -1.2 0.014 -0.7 FN -3.7

3 4 / 3 B 0.0818 -0.6 0.0463 -0.2 3 4 / 3 B 0.0147 -0.5

4 x 9 / 6 A 18.5 0.8 0.1 0.1 0.0718 1.8 4 x 9 / 6 A 0.926 0.1 0.016 -0.2 0.124 0.0

5 x 7 / 4 B 0.0473 -0.2 5 x 7 / 4 B 0.4327 -2.1 0.0241 1.7 0.0829 -1.3

6 9 / 6 A 14.6 -0.2 0.107 0.4 0.0485 -0.1 6 9 / 6 A 0.95 0.2 0.0127 -1.0 0.115 -0.3

7 x 4 / 3 B 0.113 0.7 0.0335 -1.3 7 x 4 / 3 B 0.0157 -0.3

8 x 9 / 6 A 16.4 0.3 0.111 0.6 0.0466 -0.2 8 x 9 / 6 A 0.924 0.1 0.0151 -0.4 0.12 -0.1

10 9 / 6 A 14.8 -0.1 0.0464 -2.1 0.0213 -2.3 10 9 / 6 A 0.999 0.4 0.0151 -0.4 0.11 -0.4

11 9 / 6 A 14.3 -0.3 0.102 0.2 0.0539 0.4 11 9 / 6 A 1.12 1.0 0.0177 0.2 0.0959 -0.9

12 x 9 / 6 A 12.8 -0.7 0.1 0.1 0.052 0.2 12 x 9 / 6 A 1.04 0.6 0.017 0.0 0.154 1.0

13 x 9 / 6 A 17.8 0.6 0.23 5.5 0.038 -0.9 13 x 9 / 6 A 1.06 0.7 0.0139 -0.7 0.301 5.7

14 9 / 6 A 14.8 -0.1 0.112 0.6 0.0701 1.7 14 9 / 6 A 0.821 -0.4 0.0181 0.3 0.12 -0.1

15 9 / 6 A 12.1 -0.8 0.0997 0.1 0.0632 1.1 15 9 / 6 A 0.733 -0.8 0.0181 0.3 0.128 0.1

16 9 / 6 A 19.3 1.0 0.072 -1.0 0.062 1.0 16 9 / 6 A 1.17 1.2 0.019 0.5 0.131 0.2

17 7 / 4 B 0.0848 -0.5 0.0426 -0.5 17 7 / 4 B 0.615 -1.3 0.0182 0.3

19 x 9 / 6 A 20.3 1.3 1.18 44.7 0.068 1.5 19 x 9 / 6 A 1.22 1.4 0.017 0.0 1.33 39.0

20 x 9 / 6 A 16.5 0.3 0.101 0.2 0.0422 -0.6 20 x 9 / 6 A 0.969 0.3 0.0144 -0.6 0.149 0.8

21 8 / 5 A 14.3 -0.3 0.048 -0.1 21 8 / 5 A 0.839 -0.3 0.016 -0.2 0.147 0.7

22 x 9 / 6 A 16.4 0.3 0.0772 -0.8 0.0406 -0.7 22 x 9 / 6 A 1.05 0.7 0.0147 -0.5 0.132 0.3

23 6 / 4 B 0.052 0.2 23 6 / 4 B 1.02 0.5 0.017 0.0 0.138 0.5

24 x 8 / 5 A 0.121 1.0 0.065 1.3 24 x 8 / 5 A 1 0.4 0.021 1.0 0.167 1.4

25 7 / 5 B 18.7 0.9 0.118 0.9 0.052 0.2 25 7 / 5 B 0.019 0.5 0.125 0.0

26 9 / 6 A 15.0 -0.1 0.085 -0.5 0.032 -1.4 26 9 / 6 A 0.65 -1.1 0.011 -1.4 0.16 1.2

27 9 / 6 A 17.3 0.5 0.084 -0.5 0.046 -0.3 27 9 / 6 A 1.02 0.5 0.01 -1.6 0.15 0.8

28 2 / 1 B 0.0565 0.6 28 2 / 1 B

29 x 9 / 6 A 23.61 2.1 0.08 -0.7 0.072 1.8 29 x 9 / 6 A 0.893 0.0 0.015 -0.4 0.089 -1.1

30 x 9 / 6 A 12.9 -0.6 0.114 0.7 0.049 0.0 30 x 9 / 6 A 1.04 0.6 0.049 7.6 0.149 0.8

31 9 / 6 A 18.0 0.7 0.075 -0.9 0.049 0.0 31 9 / 6 A 0.959 0.2 0.016 -0.2 0.108 -0.5

32 x 8 / 5 A 0.0842 -0.5 0.0455 -0.3 32 x 8 / 5 A 1.02 0.5 0.0157 -0.3 0.118 -0.2

33 9 / 6 A 11.3 -1.1 0.092 -0.2 0.0531 0.3 33 9 / 6 A 0.883 -0.1 0.017 0.0 0.118 -0.2

34 9 / 6 A 9.886 -1.4 0.105 0.3 0.047 -0.2 34 9 / 6 A 0.779 -0.5 0.016 -0.2 0.088 -1.2

35 8 / 5 A 0.04 -2.3 0.037 -1.0 35 8 / 5 A 1.23 1.4 0.011 -1.4 0.151 0.9

36 x 8 / 5 A 0.0786 -0.8 0.0496 0.0 36 x 8 / 5 A 0.721 -0.8 0.0171 0.1 0.0841 -1.3

37 9 / 6 A 16.4 0.3 0.087 -0.4 0.057 0.6 37 9 / 6 A 1.29 1.7 0.022 1.2 0.15 0.8

38 5 / 2 B 0.0483 -0.1 38 5 / 2 B 0.131 0.2

39 1 / 1 B 39 1 / 1 B 0.983 0.4

40 1 / 1 B 40 1 / 1 B 1.09 0.8

41 5 / 3 B 0.0686 1.6 41 5 / 3 B 1.17 1.2 0.0226 1.4

42 6 / 4 B 0.075 -0.9 0.038 -0.9 42 6 / 4 B 0.014 -0.7 0.111 -0.4

43 1 / 1 B 43 1 / 1 B 0.794 -0.5

44 2 / 1 B 44 2 / 1 B 1.989 4.8



Table 4-8 (cont.): Results reported and z-scores achieved by all participating laboratories for COMPULSORY compounds


38





CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

45 9 / 6 B 15.9 0.1 0.186 3.7 0.022 -2.2 45 9 / 6 B 0.736 -0.7 0.02 0.7 0.141 0.6

46 9 / 6 A 15.12 -0.1 0.106 0.4 0.047 -0.2 46 9 / 6 A 0.912 0.0 0.016 -0.2 0.095 -0.9

47 0 / 0 B 47 0 / 0 B

48 9 / 6 A 32.6 4.5 0.0792 -0.7 0.0538 0.4 48 9 / 6 A 0.713 -0.8 0.0198 0.7 0.155 1.0

49 x 9 / 6 A 21.85 1.7 0.058 -1.6 0.033 -1.3 49 x 9 / 6 A 0.756 -0.7 0.019 0.5 0.655 17.2

50 9 / 6 A 17.1 0.5 0.0988 0.1 0.0472 -0.2 50 9 / 6 A 1.31 1.8 0.0192 0.6 0.124 0.0

51 x 7 / 4 B 17.1 0.5 0.097 0.0 51 x 7 / 4 B 0.97 0.3 0.122 -0.1

52 9 / 6 A 16.2 0.2 0.101 0.2 0.052 0.2 52 9 / 6 A 0.794 -0.5 0.018 0.3 0.115 -0.3

53 6 / 3 B 0.1 0.1 0.039 -0.8 53 6 / 3 B 0.096 -0.9

54 x 9 / 6 A 15.8 0.1 0.092 -0.2 0.044 -0.4 54 x 9 / 6 A 1.21 1.4 0.014 -0.7 0.126 0.1

55 9 / 6 A 12.9 -0.6 0.11 0.5 0.052 0.2 55 9 / 6 A 0.667 -1.0 0.019 0.5 0.133 0.3

56 9 / 6 A 13.1 -0.6 0.119 0.9 0.0613 1.0 56 9 / 6 A 0.916 0.1 0.023 1.5 0.103 -0.7

57 x 3 / 2 B 0.104 0.3 57 x 3 / 2 B 0.148 0.8

58 1 / 1 B 58 1 / 1 B 0.867 -0.2

59 0 / 0 B 59 0 / 0 B

60 8 / 5 A 0.117 0.8 0.0507 0.1 60 8 / 5 A 0.772 -0.6 0.0137 -0.7 0.12 -0.1

61 x 8 / 5 A 0.116 0.8 0.052 0.2 61 x 8 / 5 A 0.987 0.4 0.017 0.0 0.142 0.6

62 7 / 4 B 20.0 1.2 0.0446 -2.2 0.0413 -0.6 62 7 / 4 B 0.0117 -1.2

63 9 / 6 A 13.63 -0.4 0.103 0.3 0.053 0.3 63 9 / 6 A 0.68 -1.0 0.0155 -0.3 0.021 -3.3

64 2 / 1 B 64 2 / 1 B 0.751 -0.7

65 8 / 5 A FN -3.5 0.073 -1.0 0.054 0.4 65 8 / 5 A 0.65 -1.1 0.018 0.3 0.115 -0.3

66 5 / 2 B 0.054 0.4 66 5 / 2 B 0.023 1.5 FN -3.7

67 7 / 5 B 14.1 -0.3 0.0379 -2.4 0.0345 -1.2 67 7 / 5 B 1.09 0.8 0.108 -0.5

68 x 8 / 5 A 13.7 -0.4 0.143 1.9 0.043 -0.5 68 x 8 / 5 A 0.0058 -2.6 0.173 1.6

69 9 / 6 A 13.7 -0.4 0.095 -0.1 0.047 -0.2 69 9 / 6 A 0.849 -0.2 0.014 -0.7 0.107 -0.5

70 3 / 2 B 70 3 / 2 B 0.962 0.3 0.128 0.1

71 8 / 5 A 0.0996 0.1 0.0516 0.2 71 8 / 5 A 0.788 -0.5 0.014 -0.7 0.112 -0.4

72 9 / 6 A 14.1 -0.3 0.0894 -0.3 0.0431 -0.5 72 9 / 6 A 0.896 0.0 0.0164 -0.1 0.093 -1.0

73 8 / 5 A 0.22 5.1 0.074 2.0 73 8 / 5 A 0.833 -0.3 0.022 1.2 0.127 0.1

74 x 9 / 6 A 4.29 -2.9 0.0472 -2.1 0.0431 -0.5 74 x 9 / 6 A 0.56 -1.5 0.0168 0.0 0.133 0.3

76 x 8 / 5 A 0.0716 -1.0 0.0287 -1.7 76 x 8 / 5 A 0.69 -0.9 0.0166 -0.1 0.0657 -1.9

77 x 3 / 2 B 0.084 -0.5 77 x 3 / 2 B 0.122 -0.1

78 x 9 / 6 A 12.4 -0.8 0.045 -2.1 0.055 0.5 78 x 9 / 6 A 0.722 -0.8 0.025 1.9 0.109 -0.5

79 x 9 / 6 A 12.5 -0.7 0.094 -0.1 0.05 0.1 79 x 9 / 6 A 1.182 1.2 0.015 -0.4 0.11 -0.4

80 x 6 / 4 B 0.062 1.0 80 x 6 / 4 B 2.3 6.2 0.025 1.9 0.131 0.2

82 3 / 2 B 17.0 0.4 0.096 0.0 82 3 / 2 B

83 9 / 6 A 3.0 -3.2 0.104 0.3 0.047 -0.2 83 9 / 6 A 0.48 -1.9 0.016 -0.2 0.028 -3.1

84 4 / 3 B 0.12 1.0 0.069 1.6 84 4 / 3 B 0.017 0.0

85 8 / 5 A 9.0 -1.7 0.132 1.4 0.038 -0.9 85 8 / 5 A 0.02 0.7 0.185 2.0

86 8 / 5 A 0.116 0.8 0.0538 0.4 86 8 / 5 A 0.896 0.0 0.0236 1.6 0.165 1.3

87 8 / 5 A 0.0898 -0.3 0.0451 -0.3 87 8 / 5 A 0.692 -0.9 0.017 0.0 0.111 -0.4

88 9 / 6 A 16.9 0.4 0.0263 -2.9 0.048 -0.1 88 9 / 6 A 1.1 0.9 0.014 -0.7 0.104 -0.6

89 9 / 6 A 16.5 0.3 0.081 -0.7 0.051 0.1 89 9 / 6 A 0.931 0.1 0.015 -0.4 0.075 -1.6




39

Resu

lts

4





CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

45 9 / 6 B 15.9 0.1 0.186 3.7 0.022 -2.2 45 9 / 6 B 0.736 -0.7 0.02 0.7 0.141 0.6

46 9 / 6 A 15.12 -0.1 0.106 0.4 0.047 -0.2 46 9 / 6 A 0.912 0.0 0.016 -0.2 0.095 -0.9

47 0 / 0 B 47 0 / 0 B

48 9 / 6 A 32.6 4.5 0.0792 -0.7 0.0538 0.4 48 9 / 6 A 0.713 -0.8 0.0198 0.7 0.155 1.0

49 x 9 / 6 A 21.85 1.7 0.058 -1.6 0.033 -1.3 49 x 9 / 6 A 0.756 -0.7 0.019 0.5 0.655 17.2

50 9 / 6 A 17.1 0.5 0.0988 0.1 0.0472 -0.2 50 9 / 6 A 1.31 1.8 0.0192 0.6 0.124 0.0

51 x 7 / 4 B 17.1 0.5 0.097 0.0 51 x 7 / 4 B 0.97 0.3 0.122 -0.1

52 9 / 6 A 16.2 0.2 0.101 0.2 0.052 0.2 52 9 / 6 A 0.794 -0.5 0.018 0.3 0.115 -0.3

53 6 / 3 B 0.1 0.1 0.039 -0.8 53 6 / 3 B 0.096 -0.9

54 x 9 / 6 A 15.8 0.1 0.092 -0.2 0.044 -0.4 54 x 9 / 6 A 1.21 1.4 0.014 -0.7 0.126 0.1

55 9 / 6 A 12.9 -0.6 0.11 0.5 0.052 0.2 55 9 / 6 A 0.667 -1.0 0.019 0.5 0.133 0.3

56 9 / 6 A 13.1 -0.6 0.119 0.9 0.0613 1.0 56 9 / 6 A 0.916 0.1 0.023 1.5 0.103 -0.7

57 x 3 / 2 B 0.104 0.3 57 x 3 / 2 B 0.148 0.8

58 1 / 1 B 58 1 / 1 B 0.867 -0.2

59 0 / 0 B 59 0 / 0 B

60 8 / 5 A 0.117 0.8 0.0507 0.1 60 8 / 5 A 0.772 -0.6 0.0137 -0.7 0.12 -0.1

61 x 8 / 5 A 0.116 0.8 0.052 0.2 61 x 8 / 5 A 0.987 0.4 0.017 0.0 0.142 0.6

62 7 / 4 B 20.0 1.2 0.0446 -2.2 0.0413 -0.6 62 7 / 4 B 0.0117 -1.2

63 9 / 6 A 13.63 -0.4 0.103 0.3 0.053 0.3 63 9 / 6 A 0.68 -1.0 0.0155 -0.3 0.021 -3.3

64 2 / 1 B 64 2 / 1 B 0.751 -0.7

65 8 / 5 A FN -3.5 0.073 -1.0 0.054 0.4 65 8 / 5 A 0.65 -1.1 0.018 0.3 0.115 -0.3

66 5 / 2 B 0.054 0.4 66 5 / 2 B 0.023 1.5 FN -3.7

67 7 / 5 B 14.1 -0.3 0.0379 -2.4 0.0345 -1.2 67 7 / 5 B 1.09 0.8 0.108 -0.5

68 x 8 / 5 A 13.7 -0.4 0.143 1.9 0.043 -0.5 68 x 8 / 5 A 0.0058 -2.6 0.173 1.6

69 9 / 6 A 13.7 -0.4 0.095 -0.1 0.047 -0.2 69 9 / 6 A 0.849 -0.2 0.014 -0.7 0.107 -0.5

70 3 / 2 B 70 3 / 2 B 0.962 0.3 0.128 0.1

71 8 / 5 A 0.0996 0.1 0.0516 0.2 71 8 / 5 A 0.788 -0.5 0.014 -0.7 0.112 -0.4

72 9 / 6 A 14.1 -0.3 0.0894 -0.3 0.0431 -0.5 72 9 / 6 A 0.896 0.0 0.0164 -0.1 0.093 -1.0

73 8 / 5 A 0.22 5.1 0.074 2.0 73 8 / 5 A 0.833 -0.3 0.022 1.2 0.127 0.1

74 x 9 / 6 A 4.29 -2.9 0.0472 -2.1 0.0431 -0.5 74 x 9 / 6 A 0.56 -1.5 0.0168 0.0 0.133 0.3

76 x 8 / 5 A 0.0716 -1.0 0.0287 -1.7 76 x 8 / 5 A 0.69 -0.9 0.0166 -0.1 0.0657 -1.9

77 x 3 / 2 B 0.084 -0.5 77 x 3 / 2 B 0.122 -0.1

78 x 9 / 6 A 12.4 -0.8 0.045 -2.1 0.055 0.5 78 x 9 / 6 A 0.722 -0.8 0.025 1.9 0.109 -0.5

79 x 9 / 6 A 12.5 -0.7 0.094 -0.1 0.05 0.1 79 x 9 / 6 A 1.182 1.2 0.015 -0.4 0.11 -0.4

80 x 6 / 4 B 0.062 1.0 80 x 6 / 4 B 2.3 6.2 0.025 1.9 0.131 0.2

82 3 / 2 B 17.0 0.4 0.096 0.0 82 3 / 2 B

83 9 / 6 A 3.0 -3.2 0.104 0.3 0.047 -0.2 83 9 / 6 A 0.48 -1.9 0.016 -0.2 0.028 -3.1

84 4 / 3 B 0.12 1.0 0.069 1.6 84 4 / 3 B 0.017 0.0

85 8 / 5 A 9.0 -1.7 0.132 1.4 0.038 -0.9 85 8 / 5 A 0.02 0.7 0.185 2.0

86 8 / 5 A 0.116 0.8 0.0538 0.4 86 8 / 5 A 0.896 0.0 0.0236 1.6 0.165 1.3

87 8 / 5 A 0.0898 -0.3 0.0451 -0.3 87 8 / 5 A 0.692 -0.9 0.017 0.0 0.111 -0.4

88 9 / 6 A 16.9 0.4 0.0263 -2.9 0.048 -0.1 88 9 / 6 A 1.1 0.9 0.014 -0.7 0.104 -0.6

89 9 / 6 A 16.5 0.3 0.081 -0.7 0.051 0.1 89 9 / 6 A 0.931 0.1 0.015 -0.4 0.075 -1.6




40





CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

90 1 / 0 B FN -3.6 90 1 / 0 B

91 9 / 6 A 12.4 -0.8 0.108 0.5 0.0579 0.7 91 9 / 6 A 1.01 0.5 0.0142 -0.6 0.149 0.8

92 9 / 6 A 12.9 -0.6 0.115 0.7 0.0403 -0.7 92 9 / 6 A 0.967 0.3 0.014 -0.7 0.137 0.4

93 9 / 6 A 13.0 -0.6 0.111 0.6 0.055 0.5 93 9 / 6 A 0.82 -0.4 0.018 0.3 0.15 0.8

94 1 / 1 B 18.473 0.8 94 1 / 1 B

95 1 / 1 B 95 1 / 1 B 0.121 -0.1

96 7 / 5 B 0.0895 -0.3 0.058 0.7 96 7 / 5 B 0.954 0.2 0.0166 -0.1 0.0986 -0.8

97 9 / 6 A 27.9 3.3 0.102 0.2 0.048 -0.1 97 9 / 6 A 0.832 -0.3 0.019 0.5 0.027 -3.1

98 9 / 6 A 11.6 -1.0 0.084 -0.5 0.054 0.4 98 9 / 6 A 0.859 -0.2 0.018 0.3 0.125 0.0

99 2 / 1 B 99 2 / 1 B 0.115 -0.3

100 x 4 / 3 B 16.3 0.2 0.049 0.0 100 x 4 / 3 B 0.019 0.5

101 8 / 5 A 0.101 0.2 0.025 -2.0 101 8 / 5 A 1.038 0.6 0.009 -1.9 0.198 2.4

102 1 / 1 B 7.82 -2.0 102 1 / 1 B

103 1 / 1 B 103 1 / 1 B 13.5 55.8

104 9 / 6 A 23.0 2.0 0.075 -0.9 0.025 -2.0 104 9 / 6 A 0.678 -1.0 0.012 -1.2 0.11 -0.4

105 9 / 6 A 10.3 -1.3 0.088 -0.4 0.041 -0.7 105 9 / 6 A 0.366 -2.4 0.0071 -2.3 0.19 2.1

106 5 / 3 B 0.94 34.8 106 5 / 3 B 0.93 0.1 0.1 -0.8

107 6 / 4 B 0.06 0.9 107 6 / 4 B 0.93 0.1 0.02 0.7 0.09 -1.1

109 8 / 5 A 0.168 2.9 0.0451 -0.3 109 8 / 5 A 0.824 -0.3 0.0199 0.7 0.122 -0.1

110 4 / 2 B 110 4 / 2 B 0.55 -1.6 0.143 0.6

111 4 / 2 B 19.9 1.2 111 4 / 2 B 0.089 -1.1

112 9 / 6 A 12.0 -0.9 0.12 1.0 0.06 0.9 112 9 / 6 A 0.85 -0.2 0.02 0.7 0.117 -0.2

113 0 / 0 B 113 0 / 0 B

114 0 / 0 B 114 0 / 0 B

3rd-115 6 / 3 B 0.087 -0.4 3rd-115 6 / 3 B 1.07 0.7 FN -3.3 0.123 0.0

3rd-116 8 / 5 B 12.9 -0.6 0.07 -1.1 3rd-116 8 / 5 B 0.6 -1.3 0.007 -2.3 0.11 -0.4

3rd-117 9 / 6 A 15.8 0.1 0.0689 -1.2 0.0433 -0.5 3rd-117 9 / 6 A 0.175 -3.2 0.0119 -1.2 0.152 0.9

3rd-118 6 / 3 B 14.4 -0.2 0.0831 -0.6 FN -3.2 3rd-118 6 / 3 B 0.715 -0.8

3rd-119 2 / 1 B 0.0407 -0.7 3rd-119 2 / 1 B

3rd-120 3 / 1 B 3rd-120 3 / 1 B 0.9 0.0

3rd-121 1 / 1 B 3rd-121 1 / 1 B 0.919 0.1

3rd-122 7 / 5 B 16.8 0.4 0.147 2.1 3rd-122 7 / 5 B 0.903 0.0 0.019 0.5 0.27 4.7




41

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4





CV* 24.0 % 23.5 % 20.3 % CV* 22.6 % 20.4 % 22.9 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

90 1 / 0 B FN -3.6 90 1 / 0 B

91 9 / 6 A 12.4 -0.8 0.108 0.5 0.0579 0.7 91 9 / 6 A 1.01 0.5 0.0142 -0.6 0.149 0.8

92 9 / 6 A 12.9 -0.6 0.115 0.7 0.0403 -0.7 92 9 / 6 A 0.967 0.3 0.014 -0.7 0.137 0.4

93 9 / 6 A 13.0 -0.6 0.111 0.6 0.055 0.5 93 9 / 6 A 0.82 -0.4 0.018 0.3 0.15 0.8

94 1 / 1 B 18.473 0.8 94 1 / 1 B

95 1 / 1 B 95 1 / 1 B 0.121 -0.1

96 7 / 5 B 0.0895 -0.3 0.058 0.7 96 7 / 5 B 0.954 0.2 0.0166 -0.1 0.0986 -0.8

97 9 / 6 A 27.9 3.3 0.102 0.2 0.048 -0.1 97 9 / 6 A 0.832 -0.3 0.019 0.5 0.027 -3.1

98 9 / 6 A 11.6 -1.0 0.084 -0.5 0.054 0.4 98 9 / 6 A 0.859 -0.2 0.018 0.3 0.125 0.0

99 2 / 1 B 99 2 / 1 B 0.115 -0.3

100 x 4 / 3 B 16.3 0.2 0.049 0.0 100 x 4 / 3 B 0.019 0.5

101 8 / 5 A 0.101 0.2 0.025 -2.0 101 8 / 5 A 1.038 0.6 0.009 -1.9 0.198 2.4

102 1 / 1 B 7.82 -2.0 102 1 / 1 B

103 1 / 1 B 103 1 / 1 B 13.5 55.8

104 9 / 6 A 23.0 2.0 0.075 -0.9 0.025 -2.0 104 9 / 6 A 0.678 -1.0 0.012 -1.2 0.11 -0.4

105 9 / 6 A 10.3 -1.3 0.088 -0.4 0.041 -0.7 105 9 / 6 A 0.366 -2.4 0.0071 -2.3 0.19 2.1

106 5 / 3 B 0.94 34.8 106 5 / 3 B 0.93 0.1 0.1 -0.8

107 6 / 4 B 0.06 0.9 107 6 / 4 B 0.93 0.1 0.02 0.7 0.09 -1.1

109 8 / 5 A 0.168 2.9 0.0451 -0.3 109 8 / 5 A 0.824 -0.3 0.0199 0.7 0.122 -0.1

110 4 / 2 B 110 4 / 2 B 0.55 -1.6 0.143 0.6

111 4 / 2 B 19.9 1.2 111 4 / 2 B 0.089 -1.1

112 9 / 6 A 12.0 -0.9 0.12 1.0 0.06 0.9 112 9 / 6 A 0.85 -0.2 0.02 0.7 0.117 -0.2

113 0 / 0 B 113 0 / 0 B

114 0 / 0 B 114 0 / 0 B

3rd-115 6 / 3 B 0.087 -0.4 3rd-115 6 / 3 B 1.07 0.7 FN -3.3 0.123 0.0

3rd-116 8 / 5 B 12.9 -0.6 0.07 -1.1 3rd-116 8 / 5 B 0.6 -1.3 0.007 -2.3 0.11 -0.4

3rd-117 9 / 6 A 15.8 0.1 0.0689 -1.2 0.0433 -0.5 3rd-117 9 / 6 A 0.175 -3.2 0.0119 -1.2 0.152 0.9

3rd-118 6 / 3 B 14.4 -0.2 0.0831 -0.6 FN -3.2 3rd-118 6 / 3 B 0.715 -0.8

3rd-119 2 / 1 B 0.0407 -0.7 3rd-119 2 / 1 B

3rd-120 3 / 1 B 3rd-120 3 / 1 B 0.9 0.0

3rd-121 1 / 1 B 3rd-121 1 / 1 B 0.919 0.1

3rd-122 7 / 5 B 16.8 0.4 0.147 2.1 3rd-122 7 / 5 B 0.903 0.0 0.019 0.5 0.27 4.7




42

Table 4-9: Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds

COMPULSORY Compound 2,4-DB Glufosinate MPP N-Acetyl- Glyphosate

COMPULSORY Compound Perchlorate Phosphonic acid Quizalofop Diquat

MRRL [mg/kg] 0.01 0.02 0.02 0.02 MRRL [mg/kg] 0.01 0.05 0.01 0.02

Assigned Value [mg/kg] 0.183 0.192 0.188 0.835 Assigned Value [mg/kg] 0.100 1.864 0.052 1.701 (uncertain)

CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

1 7 / 2 A 0.231 1.0 1 7 / 2 A 0.0455 -0.5 1.2 -1.2

2 12 / 5 B 0.174 -0.2 0.137 -1.1 2 12 / 5 B FN -3.6 0.142 -3.7 0.083 2.4 2.94 2.9

3 4 / 1 B 0.146 -0.8 3 4 / 1 B 0.054 0.2

4 x 9 / 5 A 0.187 -0.1 0.862 0.1 4 x 9 / 5 A 0.101 0.1 2.38 1.1 0.0572 0.4

5 x 4 / 1 B 5 x 4 / 1 B 0.0842 -0.6

6 6 / 3 A 6 6 / 3 A 0.115 0.6 1.973 0.2

7 x 4 / 1 B 0.1557 -0.6 7 x 4 / 1 B 0.0395 -1.0

8 x 6 / 3 A 0.156 -0.6 0.644 -0.9 8 x 6 / 3 A 0.113 0.5 0.0377 -1.1

10 7 / 3 A 10 7 / 3 A 0.0996 0.0 0.902 -2.1

11 10 / 4 A 0.225 0.9 11 10 / 4 A 0.0915 -0.3 FN -3.9

12 x 6 / 2 A 0.16 -0.5 0.803 -0.2 12 x 6 / 2 A 0.055 0.2

13 x 13 / 8 A 0.285 2.2 0.194 0.1 0.215 0.6 0.784 -0.2 13 x 13 / 8 A 0.109 0.4 2.36 1.1 0.0557 0.3 7.59 13.8

14 14 / 8 A 0.192 0.2 0.131 -1.3 14 14 / 8 A 0.104 0.2 1.59 -0.6 0.0512 -0.1 1.39 -0.7

15 11 / 6 A 0.261 1.4 0.173 -0.3 0.613 -1.1 15 11 / 6 A 0.0726 -1.1 2.01 0.3

16 12 / 7 A 0.219 0.8 0.286 2.0 16 12 / 7 A 0.093 -0.3 1.6 -0.6 0.066 1.1

17 9 / 6 B 0.0687 -2.6 17 9 / 6 B 0.0763 -0.9 1.94 0.2 0.0546 0.2

19 x 4 / 1 A 0.232 1.1 19 x 4 / 1 A 0.065 1.0

20 x 4 / 2 A 0.157 -0.6 20 x 4 / 2 A 0.0968 -0.1 0.0437 -0.6

21 7 / 2 A 0.863 0.1 21 7 / 2 A 0.043 -0.7 0.529 -2.8

22 x 5 / 2 A 0.2 0.4 0.198 0.1 22 x 5 / 2 A

23 4 / 1 B 0.2 0.4 23 4 / 1 B 0.056 0.3

24 x 3 / 1 A 0.19 0.2 24 x 3 / 1 A 0.059 0.5

25 2 / 0 B 25 2 / 0 B

26 8 / 5 A 0.14 -0.9 0.16 -0.7 26 8 / 5 A 0.16 2.4 2.2 0.7 0.023 -2.2

27 13 / 6 A 0.24 1.0 0.17 -0.4 27 13 / 6 A 0.12 0.8 1.623 -0.5 0.03 -1.7 2.44 1.7

28 0 / 0 B 28 0 / 0 B

29 x 2 / 0 A 29 x 2 / 0 A 0.071 1.5

30 x 15 / 8 A 0.203 0.4 0.189 -0.1 0.189 0.0 1.18 1.7 30 x 15 / 8 A 0.093 -0.3 2.05 0.4 0.062 0.8 1.35 -0.8

31 10 / 4 A 31 10 / 4 A 0.092 -0.3 1.47 -0.8 0.878 -1.9

32 x 13 / 7 A 0.142 -0.9 32 x 13 / 7 A 0.096 -0.1 1.98 0.2 0.0515 0.0 1.59 -0.3

33 10 / 5 A 0.218 0.8 0.18 -0.2 33 10 / 5 A 0.097 -0.1 1.91 0.1 0.061 0.7

34 17 / 10 A 0.176 -0.2 0.201 0.2 0.181 -0.1 16.685 76.0 34 17 / 10 A 0.089 -0.4 1.982 0.3 0.058 0.5 1.979 0.7

35 12 / 7 A 0.131 -1.1 0.183 -0.2 0.307 2.5 35 12 / 7 A 0.048 -2.1 1.278 -1.3 0.037 -1.1 1.563 -0.3

36 x 13 / 8 A 0.197 0.3 0.154 -0.8 0.171 -0.4 0.733 -0.5 36 x 13 / 8 A 0.0728 -1.1 1.65 -0.5 0.0505 -0.1 0.742 -2.3

37 8 / 5 A 0.24 1.0 0.19 0.0 37 8 / 5 A 0.11 0.4 2.04 0.4

38 3 / 1 B 38 3 / 1 B 0.102 0.1 0.0499 -0.2

39 0 / 0 B 39 0 / 0 B

40 1 / 0 B 40 1 / 0 B

41 8 / 6 B 0.217 0.7 0.23 0.8 0.159 -0.6 0.743 -0.4 41 8 / 6 B 7.5 12.1 0.0713 1.5

42 2 / 0 B 42 2 / 0 B 0.052 0.0

43 1 / 0 B 43 1 / 0 B

* Category A/B classification (Cat A was assigned to laboratories that have correctly analysed at least 8 of 9 compulsory compounds on the Target Pesti-cides List, corretly detected 5 or more out of the 6 compulsory compounds and that have not reported any false positive results)FN* = analysed for a compound present in the test material and reported not detected due to lab’s RL > assigned value, therefore judged as



43

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4

Table 4-9 (cont.): Results reported and z-scores achieved by all participating laboratories for OPTIONAL compounds





CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

1 7 / 2 A 0.231 1.0 1 7 / 2 A 0.0455 -0.5 1.2 -1.2

2 12 / 5 B 0.174 -0.2 0.137 -1.1 2 12 / 5 B FN -3.6 0.142 -3.7 0.083 2.4 2.94 2.9

3 4 / 1 B 0.146 -0.8 3 4 / 1 B 0.054 0.2

4 x 9 / 5 A 0.187 -0.1 0.862 0.1 4 x 9 / 5 A 0.101 0.1 2.38 1.1 0.0572 0.4

5 x 4 / 1 B 5 x 4 / 1 B 0.0842 -0.6

6 6 / 3 A 6 6 / 3 A 0.115 0.6 1.973 0.2

7 x 4 / 1 B 0.1557 -0.6 7 x 4 / 1 B 0.0395 -1.0

8 x 6 / 3 A 0.156 -0.6 0.644 -0.9 8 x 6 / 3 A 0.113 0.5 0.0377 -1.1

10 7 / 3 A 10 7 / 3 A 0.0996 0.0 0.902 -2.1

11 10 / 4 A 0.225 0.9 11 10 / 4 A 0.0915 -0.3 FN -3.9

12 x 6 / 2 A 0.16 -0.5 0.803 -0.2 12 x 6 / 2 A 0.055 0.2

13 x 13 / 8 A 0.285 2.2 0.194 0.1 0.215 0.6 0.784 -0.2 13 x 13 / 8 A 0.109 0.4 2.36 1.1 0.0557 0.3 7.59 13.8

14 14 / 8 A 0.192 0.2 0.131 -1.3 14 14 / 8 A 0.104 0.2 1.59 -0.6 0.0512 -0.1 1.39 -0.7

15 11 / 6 A 0.261 1.4 0.173 -0.3 0.613 -1.1 15 11 / 6 A 0.0726 -1.1 2.01 0.3

16 12 / 7 A 0.219 0.8 0.286 2.0 16 12 / 7 A 0.093 -0.3 1.6 -0.6 0.066 1.1

17 9 / 6 B 0.0687 -2.6 17 9 / 6 B 0.0763 -0.9 1.94 0.2 0.0546 0.2

19 x 4 / 1 A 0.232 1.1 19 x 4 / 1 A 0.065 1.0

20 x 4 / 2 A 0.157 -0.6 20 x 4 / 2 A 0.0968 -0.1 0.0437 -0.6

21 7 / 2 A 0.863 0.1 21 7 / 2 A 0.043 -0.7 0.529 -2.8

22 x 5 / 2 A 0.2 0.4 0.198 0.1 22 x 5 / 2 A

23 4 / 1 B 0.2 0.4 23 4 / 1 B 0.056 0.3

24 x 3 / 1 A 0.19 0.2 24 x 3 / 1 A 0.059 0.5

25 2 / 0 B 25 2 / 0 B

26 8 / 5 A 0.14 -0.9 0.16 -0.7 26 8 / 5 A 0.16 2.4 2.2 0.7 0.023 -2.2

27 13 / 6 A 0.24 1.0 0.17 -0.4 27 13 / 6 A 0.12 0.8 1.623 -0.5 0.03 -1.7 2.44 1.7

28 0 / 0 B 28 0 / 0 B

29 x 2 / 0 A 29 x 2 / 0 A 0.071 1.5

30 x 15 / 8 A 0.203 0.4 0.189 -0.1 0.189 0.0 1.18 1.7 30 x 15 / 8 A 0.093 -0.3 2.05 0.4 0.062 0.8 1.35 -0.8

31 10 / 4 A 31 10 / 4 A 0.092 -0.3 1.47 -0.8 0.878 -1.9

32 x 13 / 7 A 0.142 -0.9 32 x 13 / 7 A 0.096 -0.1 1.98 0.2 0.0515 0.0 1.59 -0.3

33 10 / 5 A 0.218 0.8 0.18 -0.2 33 10 / 5 A 0.097 -0.1 1.91 0.1 0.061 0.7

34 17 / 10 A 0.176 -0.2 0.201 0.2 0.181 -0.1 16.685 76.0 34 17 / 10 A 0.089 -0.4 1.982 0.3 0.058 0.5 1.979 0.7

35 12 / 7 A 0.131 -1.1 0.183 -0.2 0.307 2.5 35 12 / 7 A 0.048 -2.1 1.278 -1.3 0.037 -1.1 1.563 -0.3

36 x 13 / 8 A 0.197 0.3 0.154 -0.8 0.171 -0.4 0.733 -0.5 36 x 13 / 8 A 0.0728 -1.1 1.65 -0.5 0.0505 -0.1 0.742 -2.3

37 8 / 5 A 0.24 1.0 0.19 0.0 37 8 / 5 A 0.11 0.4 2.04 0.4

38 3 / 1 B 38 3 / 1 B 0.102 0.1 0.0499 -0.2

39 0 / 0 B 39 0 / 0 B

40 1 / 0 B 40 1 / 0 B

41 8 / 6 B 0.217 0.7 0.23 0.8 0.159 -0.6 0.743 -0.4 41 8 / 6 B 7.5 12.1 0.0713 1.5

42 2 / 0 B 42 2 / 0 B 0.052 0.0

43 1 / 0 B 43 1 / 0 B




44






CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

44 6 / 2 B 0.319 2.7 44 6 / 2 B 0.138 1.5

45 15 / 7 B 0.194 0.2 0.24 1.0 1.08 19.0 FN -3.9 45 15 / 7 B 0.143 1.7 1.17 -1.5 0.07 1.4 2.62 2.2

46 15 / 8 A 0.182 0.0 0.174 -0.4 0.17 -0.4 0.71 -0.6 46 15 / 8 A 0.102 0.1 1.93 0.1 0.049 -0.2 5.07 7.9

47 1 / 0 B 47 1 / 0 B FN -4.0

48 8 / 3 A 48 8 / 3 A 0.0892 -0.4 2.07 0.4 0.0463 -0.4

49 x 2 / 1 A 0.164 -0.4 49 x 2 / 1 A 0.057 0.4

50 8 / 4 A 0.183 0.0 50 8 / 4 A 0.101 0.1 2.29 0.9

51 x 0 / 0 B 51 x 0 / 0 B

52 13 / 7 A 0.216 0.7 0.205 0.3 0.225 0.8 52 13 / 7 A 0.11 0.4 1.84 -0.1 0.0504 -0.1 3.116 3.3

53 1 / 0 B 53 1 / 0 B

54 x 4 / 0 A 54 x 4 / 0 A 0.04 -0.9

55 8 / 2 A FN -3.8 FN -3.6 FN -3.9 55 8 / 2 A 1.4 -1.0 0.056 0.3

56 4 / 1 A 56 4 / 1 A 0.098 -0.1 0.0596 0.6

57 x 3 / 1 B 57 x 3 / 1 B 0.102 0.1

58 1 / 0 B 58 1 / 0 B

59 1 / 0 B 59 1 / 0 B

60 9 / 4 A 0.176 -0.2 0.172 -0.4 0.165 -0.5 60 9 / 4 A 0.0925 -0.3 0.0502 -0.1

61 x 2 / 0 A 61 x 2 / 0 A

62 9 / 5 B 0.371 3.7 62 9 / 5 B 0.115 0.6 1.96 0.2 0.0568 0.4 0.864 -2.0

63 15 / 8 A 0.19 0.2 0.7 10.6 0.156 -0.7 0.769 -0.3 63 15 / 8 A 0.033 -2.7 0.387 -3.2 0.044 -0.6 0.43 -3.0

64 2 / 0 B 64 2 / 0 B

65 2 / 0 A 65 2 / 0 A

66 2 / 0 B 66 2 / 0 B FN -3.2

67 9 / 5 B 0.177 -0.3 0.173 -0.3 67 9 / 5 B 0.0825 -0.7 1.95 0.2 0.0301 -1.7

68 x 2 / 0 A 68 x 2 / 0 A

69 8 / 4 A 0.234 1.1 69 8 / 4 A 0.193 3.7 1.86 0.0 0.046 -0.5

70 0 / 0 B 70 0 / 0 B

71 11 / 5 A 0.155 -0.6 0.203 0.2 0.977 0.7 71 11 / 5 A 0.117 0.7 1.25 -1.1

72 8 / 4 A 0.164 -0.4 72 8 / 4 A 0.0921 -0.3 1.75 -0.2 0.0486 -0.3

73 4 / 1 A 0.152 -0.8 73 4 / 1 A

74 x 3 / 1 A 0.139 -1.0 74 x 3 / 1 A

76 x 9 / 3 A 0.174 -0.2 0.166 -0.5 FN -3.9 76 x 9 / 3 A 0.0221 -2.3 3.48 4.2

77 x 1 / 0 B 77 x 1 / 0 B

78 x 1 / 1 A 0.133 -1.2 78 x 1 / 1 A

79 x 7 / 4 A 0.132 -1.1 0.105 -1.8 79 x 7 / 4 A 0.041 -0.8

80 x 2 / 0 B 80 x 2 / 0 B

82 2 / 0 B 82 2 / 0 B

83 15 / 8 A 0.19 0.2 0.13 -1.3 0.15 -0.8 0.65 -0.9 83 15 / 8 A 0.023 -3.1 0.37 -3.2 0.055 0.2 1.5 -0.5

84 1 / 0 B 84 1 / 0 B

85 7 / 2 A 0.173 -0.2 85 7 / 2 A 0.102 0.1 FN -3.9

86 11 / 6 A 0.319 3.0 0.224 0.7 0.979 0.7 86 11 / 6 A 2.13 0.6 0.0517 0.0 1.28 -1.0




45

Resu

lts

4






CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

44 6 / 2 B 0.319 2.7 44 6 / 2 B 0.138 1.5

45 15 / 7 B 0.194 0.2 0.24 1.0 1.08 19.0 FN -3.9 45 15 / 7 B 0.143 1.7 1.17 -1.5 0.07 1.4 2.62 2.2

46 15 / 8 A 0.182 0.0 0.174 -0.4 0.17 -0.4 0.71 -0.6 46 15 / 8 A 0.102 0.1 1.93 0.1 0.049 -0.2 5.07 7.9

47 1 / 0 B 47 1 / 0 B FN -4.0

48 8 / 3 A 48 8 / 3 A 0.0892 -0.4 2.07 0.4 0.0463 -0.4

49 x 2 / 1 A 0.164 -0.4 49 x 2 / 1 A 0.057 0.4

50 8 / 4 A 0.183 0.0 50 8 / 4 A 0.101 0.1 2.29 0.9

51 x 0 / 0 B 51 x 0 / 0 B

52 13 / 7 A 0.216 0.7 0.205 0.3 0.225 0.8 52 13 / 7 A 0.11 0.4 1.84 -0.1 0.0504 -0.1 3.116 3.3

53 1 / 0 B 53 1 / 0 B

54 x 4 / 0 A 54 x 4 / 0 A 0.04 -0.9

55 8 / 2 A FN -3.8 FN -3.6 FN -3.9 55 8 / 2 A 1.4 -1.0 0.056 0.3

56 4 / 1 A 56 4 / 1 A 0.098 -0.1 0.0596 0.6

57 x 3 / 1 B 57 x 3 / 1 B 0.102 0.1

58 1 / 0 B 58 1 / 0 B

59 1 / 0 B 59 1 / 0 B

60 9 / 4 A 0.176 -0.2 0.172 -0.4 0.165 -0.5 60 9 / 4 A 0.0925 -0.3 0.0502 -0.1

61 x 2 / 0 A 61 x 2 / 0 A

62 9 / 5 B 0.371 3.7 62 9 / 5 B 0.115 0.6 1.96 0.2 0.0568 0.4 0.864 -2.0

63 15 / 8 A 0.19 0.2 0.7 10.6 0.156 -0.7 0.769 -0.3 63 15 / 8 A 0.033 -2.7 0.387 -3.2 0.044 -0.6 0.43 -3.0

64 2 / 0 B 64 2 / 0 B

65 2 / 0 A 65 2 / 0 A

66 2 / 0 B 66 2 / 0 B FN -3.2

67 9 / 5 B 0.177 -0.3 0.173 -0.3 67 9 / 5 B 0.0825 -0.7 1.95 0.2 0.0301 -1.7

68 x 2 / 0 A 68 x 2 / 0 A

69 8 / 4 A 0.234 1.1 69 8 / 4 A 0.193 3.7 1.86 0.0 0.046 -0.5

70 0 / 0 B 70 0 / 0 B

71 11 / 5 A 0.155 -0.6 0.203 0.2 0.977 0.7 71 11 / 5 A 0.117 0.7 1.25 -1.1

72 8 / 4 A 0.164 -0.4 72 8 / 4 A 0.0921 -0.3 1.75 -0.2 0.0486 -0.3

73 4 / 1 A 0.152 -0.8 73 4 / 1 A

74 x 3 / 1 A 0.139 -1.0 74 x 3 / 1 A

76 x 9 / 3 A 0.174 -0.2 0.166 -0.5 FN -3.9 76 x 9 / 3 A 0.0221 -2.3 3.48 4.2

77 x 1 / 0 B 77 x 1 / 0 B

78 x 1 / 1 A 0.133 -1.2 78 x 1 / 1 A

79 x 7 / 4 A 0.132 -1.1 0.105 -1.8 79 x 7 / 4 A 0.041 -0.8

80 x 2 / 0 B 80 x 2 / 0 B

82 2 / 0 B 82 2 / 0 B

83 15 / 8 A 0.19 0.2 0.13 -1.3 0.15 -0.8 0.65 -0.9 83 15 / 8 A 0.023 -3.1 0.37 -3.2 0.055 0.2 1.5 -0.5

84 1 / 0 B 84 1 / 0 B

85 7 / 2 A 0.173 -0.2 85 7 / 2 A 0.102 0.1 FN -3.9

86 11 / 6 A 0.319 3.0 0.224 0.7 0.979 0.7 86 11 / 6 A 2.13 0.6 0.0517 0.0 1.28 -1.0




46






CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

87 5 / 2 A 0.146 -0.8 87 5 / 2 A 0.0679 -1.3 0.0508 -0.1

88 10 / 6 A 0.18 -0.1 0.247 1.2 0.233 1.0 88 10 / 6 A 0.11 0.4 2.12 0.5 0.052 0.0

89 15 / 6 A 0.167 -0.3 FN -3.6 0.162 -0.6 FN -3.9 89 15 / 6 A 0.102 0.1 2.24 0.8 0.052 0.0 1.45 -0.6

90 1 / 0 B 90 1 / 0 B

91 11 / 6 A 0.134 -1.1 0.215 0.6 0.72 -0.5 91 11 / 6 A 0.106 0.3 0.688 -2.5 0.0547 0.2

92 7 / 4 A 0.0954 -2.0 0.19 0.0 92 7 / 4 A 0.101 0.1 0.0332 -1.4 1.74 0.1

93 12 / 6 A 0.216 0.7 0.181 -0.2 93 12 / 6 A 0.14 1.6 2.4 1.1 0.068 1.2 1.8 0.2

94 0 / 0 B 94 0 / 0 B

95 0 / 0 B 95 0 / 0 B

96 1 / 0 B 96 1 / 0 B 0.0613 0.7

97 13 / 5 A 0.234 1.1 0.227 0.7 0.169 -0.4 97 13 / 5 A 0.099 0.0 FN -3.9 0.063 0.9 1.9 0.5

98 12 / 7 A 0.147 -0.8 0.199 0.2 98 12 / 7 A 0.102 0.1 2.45 1.3 0.054 0.2

99 1 / 0 B 99 1 / 0 B

100 x 0 / 0 B 100 x 0 / 0 B

101 14 / 7 A 0.104 -1.7 0.188 -0.1 0.617 9.1 101 14 / 7 A 0.335 9.5 2.133 0.6 0.023 -2.2 1.922 0.5

102 0 / 0 B 102 0 / 0 B

103 0 / 0 B 103 0 / 0 B

104 0 / 0 A 104 0 / 0 A

105 13 / 6 A 0.193 0.2 FN -3.6 0.066 -2.6 0.938 0.5 105 13 / 6 A 0.09 -0.4 1.67 -0.4 0.035 -1.3

106 3 / 2 B 106 3 / 2 B 2.4 1.1

107 7 / 3 B 0.16 -0.5 0.23 0.8 107 7 / 3 B 0.1 3.7 1.41 -0.7

109 12 / 1 A FN -3.8 0.114 -1.6 FN -3.6 FN -3.9 109 12 / 1 A FN -3.6 0.045 -0.5 FN -4.0

110 5 / 2 B 110 5 / 2 B 0.087 -0.5 0.768 -2.2

111 2 / 1 B 111 2 / 1 B 0.096 -0.1

112 17 / 10 A 0.24 1.2 0.185 -0.1 0.198 0.2 1.04 1.0 112 17 / 10 A 0.106 0.3 2.02 0.3 0.081 2.2 1.6 -0.2

113 2 / 2 B 113 2 / 2 B

114 2 / 2 B 114 2 / 2 B

3rd-115 5 / 2 B FN -3.8 0.183 -0.2 3rd-115 5 / 2 B FN -3.6 1.11 -1.4

3rd-116 4 / 2 B 0.166 -0.5 3rd-116 4 / 2 B 0.27 -3.4

3rd-117 5 / 2 A 0.131 -1.1 0.166 -0.5 3rd-117 5 / 2 A

3rd-118 6 / 1 B 3rd-118 6 / 1 B FN -3.6 0.913 -1.9

3rd-119 2 / 1 B 0.188 0.1 3rd-119 2 / 1 B

3rd-120 3 / 1 B 0.2 0.2 3rd-120 3 / 1 B

3rd-121 1 / 0 B FN -3.6 3rd-121 1 / 0 B

3rd-122 1 / 1 B 0.223 0.7 3rd-122 1 / 1 B




47

Resu

lts

4






CV* 20.7 % 28.7 % 18.9 % 21.1 % CV* 16.9 % 24.3 % 23.6 % 52.8 %

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Lab code

SRM13-

NRL-SRM


Cat.* Conc. [mg/kg]

z-Score § (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

Conc. [mg/kg]

z-Score (FFP-RSD

= 25 %)

87 5 / 2 A 0.146 -0.8 87 5 / 2 A 0.0679 -1.3 0.0508 -0.1

88 10 / 6 A 0.18 -0.1 0.247 1.2 0.233 1.0 88 10 / 6 A 0.11 0.4 2.12 0.5 0.052 0.0

89 15 / 6 A 0.167 -0.3 FN -3.6 0.162 -0.6 FN -3.9 89 15 / 6 A 0.102 0.1 2.24 0.8 0.052 0.0 1.45 -0.6

90 1 / 0 B 90 1 / 0 B

91 11 / 6 A 0.134 -1.1 0.215 0.6 0.72 -0.5 91 11 / 6 A 0.106 0.3 0.688 -2.5 0.0547 0.2

92 7 / 4 A 0.0954 -2.0 0.19 0.0 92 7 / 4 A 0.101 0.1 0.0332 -1.4 1.74 0.1

93 12 / 6 A 0.216 0.7 0.181 -0.2 93 12 / 6 A 0.14 1.6 2.4 1.1 0.068 1.2 1.8 0.2

94 0 / 0 B 94 0 / 0 B

95 0 / 0 B 95 0 / 0 B

96 1 / 0 B 96 1 / 0 B 0.0613 0.7

97 13 / 5 A 0.234 1.1 0.227 0.7 0.169 -0.4 97 13 / 5 A 0.099 0.0 FN -3.9 0.063 0.9 1.9 0.5

98 12 / 7 A 0.147 -0.8 0.199 0.2 98 12 / 7 A 0.102 0.1 2.45 1.3 0.054 0.2

99 1 / 0 B 99 1 / 0 B

100 x 0 / 0 B 100 x 0 / 0 B

101 14 / 7 A 0.104 -1.7 0.188 -0.1 0.617 9.1 101 14 / 7 A 0.335 9.5 2.133 0.6 0.023 -2.2 1.922 0.5

102 0 / 0 B 102 0 / 0 B

103 0 / 0 B 103 0 / 0 B

104 0 / 0 A 104 0 / 0 A

105 13 / 6 A 0.193 0.2 FN -3.6 0.066 -2.6 0.938 0.5 105 13 / 6 A 0.09 -0.4 1.67 -0.4 0.035 -1.3

106 3 / 2 B 106 3 / 2 B 2.4 1.1

107 7 / 3 B 0.16 -0.5 0.23 0.8 107 7 / 3 B 0.1 3.7 1.41 -0.7

109 12 / 1 A FN -3.8 0.114 -1.6 FN -3.6 FN -3.9 109 12 / 1 A FN -3.6 0.045 -0.5 FN -4.0

110 5 / 2 B 110 5 / 2 B 0.087 -0.5 0.768 -2.2

111 2 / 1 B 111 2 / 1 B 0.096 -0.1

112 17 / 10 A 0.24 1.2 0.185 -0.1 0.198 0.2 1.04 1.0 112 17 / 10 A 0.106 0.3 2.02 0.3 0.081 2.2 1.6 -0.2

113 2 / 2 B 113 2 / 2 B

114 2 / 2 B 114 2 / 2 B

3rd-115 5 / 2 B FN -3.8 0.183 -0.2 3rd-115 5 / 2 B FN -3.6 1.11 -1.4

3rd-116 4 / 2 B 0.166 -0.5 3rd-116 4 / 2 B 0.27 -3.4

3rd-117 5 / 2 A 0.131 -1.1 0.166 -0.5 3rd-117 5 / 2 A

3rd-118 6 / 1 B 3rd-118 6 / 1 B FN -3.6 0.913 -1.9

3rd-119 2 / 1 B 0.188 0.1 3rd-119 2 / 1 B

3rd-120 3 / 1 B 0.2 0.2 3rd-120 3 / 1 B

3rd-121 1 / 0 B FN -3.6 3rd-121 1 / 0 B

3rd-122 1 / 1 B 0.223 0.7 3rd-122 1 / 1 B




48

4.4.4 Laboratory Classification Based on Scope

All participating laboratories having reported at least one result were classified into categories A or B ac-cording to the rules stated in Section 2.5 (p. 12). Following the rules defined in the General Protocol (8th Edition, see Appendix 8), a laboratory had to fulfill the following conditions in order to be classified into Category A in the present PT: a) analysis of at least eight out of the nine compulsory pesticides on the Target Pesticides List; b) correct detection of at least five out of the six compulsory pesticides present in the test item, and c) no false positive results.

A total of 64 EU and EFTA laboratories (59 %) were classified into Category A and 45 (41 %) into Category B. One out of the 8 EU candidate and third-country laboratories was classified into Category A. Considering only the compulsory compounds the laboratories from EU and EFTA countries classified into Category A achieved an overall AAZ of 0.8 (n = 362), whereas those classified into Category B achieved an overall AAZ of 1.1 (n = 110). When including laboratories from EU candidate and third countries, the AAZ for compsul-sory compounds remains the same (n = 367) and for optional compounds decreased to 1.0 (n = 131).

Table 4-10 and Table 4-11 (p. 50) show the details of laboratories classified into Category A and B, respec-tively. For informative purposes, the overall AAZ was calculated for laboratories with 5 or more individual z-scores among the compulsory compounds. For the AAZ calculation any z-scores > 5 were set at 5.

COMPULSORY Compounds Bromide ion Cyromazine Fluazifop Glyphosate Haloxyfop Mepiquat-Cl

MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01

Assigned Value [mg/kg] 15.356 0.097 0.049 0.903 0.017 0.124

CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %

Lab code SRM13-

NRL-SRM

Analysed / corr. found 1) z-Scores z-Scores z-Scores z-Scores z-Scores z-Scores AAZ 2)

1 8 / 5 1.3 0.3 0.1 -0.2 0.0 0.4

4 x 9 / 6 0.8 0.1 1.8 0.1 -0.2 0.0 0.5

6 9 / 6 -0.2 0.4 -0.1 0.2 -1.0 -0.3 0.4

8 x 9 / 6 0.3 0.6 -0.2 0.1 -0.4 -0.1 0.3

10 9 / 6 -0.1 -2.1 -2.3 0.4 -0.4 -0.4 1.0

11 9 / 6 -0.3 0.2 0.4 1.0 0.2 -0.9 0.5

12 x 9 / 6 -0.7 0.1 0.2 0.6 0.0 1.0 0.4

13 x 9 / 6 0.6 5.5 -0.9 0.7 -0.7 5.7 2.2

14 9 / 6 -0.1 0.6 1.7 -0.4 0.3 -0.1 0.5

15 9 / 6 -0.8 0.1 1.1 -0.8 0.3 0.1 0.5

16 9 / 6 1.0 -1.0 1.0 1.2 0.5 0.2 0.8

19 x 9 / 6 1.3 44.7 1.5 1.4 0.0 39.0 2.4

20 x 9 / 6 0.3 0.2 -0.6 0.3 -0.6 0.8 0.5

21 8 / 5 -0.3 -0.1 -0.3 -0.2 0.7 0.3

22 x 9 / 6 0.3 -0.8 -0.7 0.7 -0.5 0.3 0.6

24 x 8 / 5 1.0 1.3 0.4 1.0 1.4 1.0

26 9 / 6 -0.1 -0.5 -1.4 -1.1 -1.4 1.2 1.0

27 9 / 6 0.5 -0.5 -0.3 0.5 -1.6 0.8 0.7

29 x 9 / 6 2.1 -0.7 1.8 0.0 -0.4 -1.1 1.0

30 x 9 / 6 -0.6 0.7 0.0 0.6 7.6 0.8 1.3

31 9 / 6 0.7 -0.9 0.0 0.2 -0.2 -0.5 0.41) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned

values based on the entire population. For the calculation of the AAZ the value “5” was applied where the z-score was higher than 5 (shown in square brackets).

FN = false negative results

Table 4-10: Category A laboratories ordered by lab-codes


49

Resu

lts

4


MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01


CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %

Lab code SRM13-

NRL-SRM


32 x 8 / 5 -0.5 -0.3 0.5 -0.3 -0.2 0.4

33 9 / 6 -1.1 -0.2 0.3 -0.1 0.0 -0.2 0.3

34 9 / 6 -1.4 0.3 -0.2 -0.5 -0.2 -1.2 0.6

35 8 / 5 -2.3 -1.0 1.4 -1.4 0.9 1.4

36 x 8 / 5 -0.8 0.0 -0.8 0.1 -1.3 0.6

37 9 / 6 0.3 -0.4 0.6 1.7 1.2 0.8 0.8

46 9 / 6 -0.1 0.4 -0.2 0.0 -0.2 -0.9 0.3

48 9 / 6 4.5 -0.7 0.4 -0.8 0.7 1.0 1.4

49 x 9 / 6 1.7 -1.6 -1.3 -0.7 0.5 17.2 1.8

50 9 / 6 0.5 0.1 -0.2 1.8 0.6 0.0 0.5

52 9 / 6 0.2 0.2 0.2 -0.5 0.3 -0.3 0.3

54 x 9 / 6 0.1 -0.2 -0.4 1.4 -0.7 0.1 0.5

55 9 / 6 -0.6 0.5 0.2 -1.0 0.5 0.3 0.5

56 9 / 6 -0.6 0.9 1.0 0.1 1.5 -0.7 0.8

60 8 / 5 0.8 0.1 -0.6 -0.7 -0.1 0.5

61 x 8 / 5 0.8 0.2 0.4 0.0 0.6 0.4

63 9 / 6 -0.4 0.3 0.3 -1.0 -0.3 -3.3 0.9

65 8 / 5 -3.5FN -1.0 0.4 -1.1 0.3 -0.3 1.1

68 x 8 / 5 -0.4 1.9 -0.5 -2.6 1.6 1.4

69 9 / 6 -0.4 -0.1 -0.2 -0.2 -0.7 -0.5 0.4

71 8 / 5 0.1 0.2 -0.5 -0.7 -0.4 0.4

72 9 / 6 -0.3 -0.3 -0.5 0.0 -0.1 -1.0 0.4

73 8 / 5 5.1 2.0 -0.3 1.2 0.1 1.7

74 x 9 / 6 -2.9 -2.1 -0.5 -1.5 0.0 0.3 1.2

76 x 8 / 5 -1.0 -1.7 -0.9 -0.1 -1.9 1.1

78 x 9 / 6 -0.8 -2.1 0.5 -0.8 1.9 -0.5 1.1

79 x 9 / 6 -0.7 -0.1 0.1 1.2 -0.4 -0.4 0.5

83 9 / 6 -3.2 0.3 -0.2 -1.9 -0.2 -3.1 1.5

85 8 / 5 -1.7 1.4 -0.9 0.7 2.0 1.3

86 8 / 5 0.8 0.4 0.0 1.6 1.3 0.8

87 8 / 5 -0.3 -0.3 -0.9 0.0 -0.4 0.4

88 9 / 6 0.4 -2.9 -0.1 0.9 -0.7 -0.6 0.9

89 9 / 6 0.3 -0.7 0.1 0.1 -0.4 -1.6 0.5

91 9 / 6 -0.8 0.5 0.7 0.5 -0.6 0.8 0.7

92 9 / 6 -0.6 0.7 -0.7 0.3 -0.7 0.4 0.6

93 9 / 6 -0.6 0.6 0.5 -0.4 0.3 0.8 0.5

97 9 / 6 3.3 0.2 -0.1 -0.3 0.5 -3.1 1.3

98 9 / 6 -1.0 -0.5 0.4 -0.2 0.3 0.0 0.4

101 8 / 5 0.2 -2.0 0.6 -1.9 2.4 1.4

104 9 / 6 2.0 -0.9 -2.0 -1.0 -1.2 -0.4 1.3

105 9 / 6 -1.3 -0.4 -0.7 -2.4 -2.3 2.1 1.5

109 8 / 5 2.9 -0.3 -0.3 0.7 -0.1 0.9

112 9 / 6 -0.9 1.0 0.9 -0.2 0.7 -0.2 0.7

3rd-117 9 / 6 0.1 -1.2 -0.5 -3.2 -1.2 0.9 1.21) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned



Table 4-11 (cont.): Category A laboratories ordered by lab-codes


50

Table 4-11: Category B laboratories ordered by lab-codes


MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01


CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %

Lab code SRM13-

NRL-SRM


2 9 / 4 0.0 -3.6FN 0.2 -1.2 -0.7 -3.7FN

3 4 / 3 -0.6 -0.2 -0.5

5 x 7 / 4 -0.2 -2.1 1.7 -1.3

7 x 4 / 3 0.7 -1.3 -0.3

17 7 / 4 -0.5 -0.5 -1.3 0.3

23 6 / 4 0.2 0.5 0.0 0.5

25 7 / 5 0.9 0.9 0.2 0.5 0.0 0.5

28 2 / 1 0.6

38 5 / 2 -0.1 0.2

39 1 / 1 0.4

40 1 / 1 0.8

41 5 / 3 1.6 1.2 1.4

42 6 / 4 -0.9 -0.9 -0.7 -0.4

43 1 / 1 -0.5

44 2 / 1 4.8

45 9 / 6 0.1 3.7 -2.2 -0.7 0.7 0.6 1.3

47 0 / 0

51 x 7 / 4 0.5 0.0 0.3 -0.1

53 6 / 3 0.1 -0.8 -0.9

57 x 3 / 2 0.3 0.8

58 1 / 1 -0.2

59 0 / 0

62 7 / 4 1.2 -2.2 -0.6 -1.2

64 2 / 1 -0.7

66 5 / 2 0.4 1.5 -3.7FN

67 7 / 5 -0.3 -2.4 -1.2 0.8 -0.5 1

70 3 / 2 0.3 0.1

77 x 3 / 2 -0.5 -0.1

80 x 6 / 4 1.0 6.2 1.9 0.2

82 3 / 2 0.4 0.0

84 4 / 3 1.0 1.6 0.0

90 1 / 0 -3.6FN

94 1 / 1 0.8

95 1 / 1 -0.1

96 7 / 5 -0.3 0.7 0.2 -0.1 -0.8 0.4

99 2 / 1 -0.3

100 x 4 / 3 0.2 0.0 0.5

102 1 / 1 -2.0

103 1 / 1 55.8

106 5 / 3 34.8 0.1 -0.8

107 6 / 4 0.9 0.1 0.7 -1.1

1) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned




51

Resu

lts

4


MRRL [mg/kg] 2 0.01 0.01 0.03 0.003 0.01


CV* 24.0 % 23.5 % 20.3 % 22.6 % 20.4 % 22.9 %

Lab code SRM13-

NRL-SRM


110 4 / 2 -1.6 0.6

111 4 / 2 1.2 -1.1

113 0 / 0

114 0 / 0

3rd-115 6 / 3 -0.4 0.7 -3.3FN 0.0

3rd-116 8 / 5 -0.6 -1.1 -1.3 -2.3 -0.4 1.1

3rd-118 6 / 3 -0.2 -0.6 -3.2FN -0.8

3rd-119 2 / 1 -0.7

3rd-120 3 / 1 0.0

3rd-121 1 / 1 0.1

3rd-122 7 / 5 0.4 2.1 0.0 0.5 4.7 1.51) Referring to compulsory compounds only (max. 13/8)2) AAZ: Average of Absolute z-scores, is given for informative purposes. It was calculated using all z-scores of each laboratory using assigned



Table 4-12 (cont.): Category B laboratories ordered by lab-codes

4.4.5 Feedback from Laboratories in Case of Poor Results

Like in the previous EUPT-SRMs, as a follow-up measure to this EUPT, all participating laboratories having achieved questionable (2 < |z-score| < 3) or unacceptable (|z-score| ≥ 3) results were asked to in-vestigate the reasons for their poor performance and to report them to the organisers. The aim of this measure is to sensibilize the laboratories to investigate the sources of errors. A compilation of the feedback received by the laboratories is given in Appendix 7. With this compilation it is intended to make all partici-panting labs aware of common and potential error sources so that they can be avoided or eliminated in the future. This information also provides input to NRLs on how to better assist OfLs within the network in improving their performance.

In the current PT, excluding diquat, phosphine (Test Item) and phosphine (PH3-Tube) that showed an unac-ceptble uncertainty of their assigned values, in total 821 results for the analytes present in the test items and 5 false positive results were reported by 116 participants. 98 results by 51 laboratories were allocated with |z| > 2, and thereof 63 results by 40 laboratories with |z| ≥ 3 (see Section Table 4-7, p. 35). Among EU and EFTA laboratories, |z| > 2 was assigned to 33 results by 23 laboratories, and |z| ≥ 3 to 55 results by 33 laboratories. All these laboratories and those having obtained false positive results were asked to provide a feedback. Overall, 43 laboratories responced to the organisers with (possible) reasons for their poor per-formance in 86 cases. In 7 cases the real reasons for generating biased results could not be clarified, despite of intensive investigation. The most frequently reported error sources were “lack of experience” (28 cases) and often combined with “matrix effect not properly compensated” (20 cases) and/or “use of inappropri-ate procedure” (21 cases). The current matrix “soybean flour”, a dry matrix with high content on fat (approx. 20 %) and even with starch and biological surfactant lecithin, was surely a difficult matrix and out of the routine analytical scope. Lacking of experience with soy beans, part of the participants applied in the PT


52

simply the the extraction solvents and procedures which work usually well for fruit and vegetable but not for soybeans. During the investigation a few participants observed that addition of water and soaking enhance the extraction yield (Appendix 7). Compared with the previouse EUPT-SRMs, the percentage of

“transcription error” was high in this PT (14 cases). Most of the transcription errors occured during results submission, in particular if the submission tool didn’t work correctly and one was under stress. Together with other EURLs, the organiser is working on a new, and hopefully more comfortable and stable submis-sion tool. The transcription errors occured also during typing of the concentration of the calibration solu-tion.

Other error sources commonly reported were: “error in concentration of analytical standard/calibration stock” (9 cases) or “procedure not properly conducted/error during sample preparation“ (8 cases), “inap-propriate calibration “ (4 cases), “detection signals strongly interferred by matrix components/strong chro-matographic interferences“ (each 3 cases), “misunderstanding of the definition of the analyte”, “sample weight too small, homogeneity not waranteed“, “error in the evaluation/interpretation of measurement data“, “technical problems/diffculties with measurement instrumentation“ and “contamination“ (each 2 cases) as well as “error in the conversion factor“, “sample amount not sufficient for conducting confirma-tion analysis” and “reporting limit higher than the assigned value“ (each one case). The responses from the other labratories are pending.

5. Acknowledgements / 6. References

53

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ces

5/6

5. ACkNOWLEDGEMENTS

The organisers wish to thank the members of the EUPT Scientific Committee (Quality Control Group and Advisory Group) for their valuable advice. Special thanks also go to Jens-Ole Frimann for his support in establishing the online result submission tool.

6. REFERENCES

[1] Regulation (EC) N° 882/2004 of the European Parliament and of the Council on official controls per-formed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules. Published at OJ of the EU L191 of 28.05.2004

[2] Regulation (EC) N° 396/2005, published at OJ of the EU L70 of 16.03.2005, as last amended by Regula-tion 839/2008 published at OJ of the EU L234 of 30.08.2008.

[3] http://www.crl-pesticides.eu/userfiles/file/EurlSRM/EurlSrm_Observations_AcidicPesticides.pdf

[4] Thompson M., Ellison S.L.R. and Wood R., The International Harmonized Protocol for the Proficiency Testing of Analytical Chemistry Laboratories (IUPAC Technical Report). Pure Appl. Chem., Vol. 78, No. 1, pp. 145 – 196, 2006

[5] http://quppe.eu/

[6] ISO 13528:2015: Statistical methods for use in proficiency testing by interlaboratory comparisons.

Appendix 1. List of Laboratories Registered to Participate in the EUPT-SRM13

Part

iciP

atio

n

a1

A-1

7. APPENDICES

Country (Location)

Analysed on behalf of Institution City NRL*-

SRMReported

results

Austria AT AGES Innsbruck (LSI-PLMA) Innsbruck x Yes

Belgium BE WIV-ISP (Belgian Scientific Institute of Public Health) Brussels x Yes

Belgium BE; BG; FR; LU

Primoris - Belgium Gent - Zwijnaarde Yes

Bulgaria BG CLCTC Sofia x Yes

Croatia HR Euroinspekt - Croatiakontrola Zagreb Yes

Croatia HR Inspecto d.o.o. Laboratorij Osijek (Industrijska zona Nemetin)

Yes

Croatia HR NZJZ dr.A.Štampar Zagreb Yes

Cyprus CY FP lab of S.G.L Nicosia x Yes

Czech Republic

CZ Central Institute for Supervising and Testing in Agriculture Brno Yes

Czech Republic

CZ Czech Agriculture and Food Inspection Authority Prague x Yes

Czech Republic

CZ VSCHT Praha, Analyza potravin Praha 6 Yes

Denmark DK Fodevarestyrelsen Ringsted x Yes

Estonia EE PMK, JSL Saku Yes

Estonia EE Tartu Laboratory of Health Boa Tartu x Yes

Finland FI Finnish Customs Laboratory Espoo x Yes

Finland FI Finnish Food Safety Authority Helsinki x Yes

France FR ANSES-LSAL Maisons-Alfort Cedex x Yes

France FR CAMP 66 perpignan Yes

France FR CAPINOV Landerneau Yes

France FR CERECO GARONS Yes

France FR GIRPA BEAUCOUZE Yes

France FR INOVALYS Le Mans Yes

France FR Laboratoire du SCL Montpellier Yes

France FR SCL Laboratoire de Paris Massy Cedex Yes

France BE PHYTOCONTROL NIMES Yes

Germany BE LUFA-ITL GmbH Kiel Yes

Germany DE BfUL FB 42 Nossen Yes

Germany DE Bundesamt für Verbraucherschutz und Lebensmittelsi-cherheit

Berlin-Marienfelde x Yes

Germany DE CVUA Münsterland Emscher-Lippe Münster Yes

Germany DE CVUA RRW Krefeld Yes

Germany DE Eurofins SOFIA GmbH Berlin Yes

Germany DE Institut für Hygiene und Umwel Hamburg No

Germany DE Kwalis Qualitätsforschung Fulda Dipperz Yes

Germany DE Labor Friedle GmbH Tegernheim Yes

Germany DE Landesamt für Landwirtschaft, Lebensmittelsicherheit und Fischerei

Rostock Yes

Germany DE Landesamt für Verbraucherschut Halle/Saale Yes

Germany DE Landeslabor Berlin-Brandenburg Potsdam Yes

Germany DE Landesuntersuchungsamt - ILC Speyer Speyer Yes

* only for EU-Member States

Appendix 1 List of Laboratories Registered to Participate in the EUPT-SRM13

(a): participating labs of EU and EFTA Member States


A-2

Country (Location)


SRMReported

results

Germany DE Landesuntersuchungsanstalt für das Gesundheits- und Veterinärwesen Sachsen Reichenbachstr. 71/73 01217 Dresden Germany

Dresden Yes

Germany DE LAVES Futtermittelinstitut Stade Stade Yes

Germany DE LAVES, LVI Oldenburg Oldenburg Yes

Germany DE LGL Erlangen Yes

Germany DE LLG Halle Halle/Saale Yes

Germany DE LTZ Augustenberg Karlsruhe Yes

Germany DE LUFA Speyer Speyer Yes

Germany DE Stadt Duesseldorf - Abteilung Duesseldorf Yes

Germany DE State Laboratory Schleswig-Holstein Neumünster Yes

Germany DE; MT Eurofins Dr. Specht Laboratorien GmbH Hamburg Yes

Germany LT GALAB Laboratories GmbH Hamburg Yes

Greece GR AGROLAB-RDS Thessaloniki Yes

Greece GR Benaki Pesticide Residue Labor Kifissia x Yes

Greece GR General Chemical State Laboratory, A Chemical Division, Pesticide Residues Laboratory

Athens x Yes

Hungary HU Food Chain Safety Centre Non-profit Ltd. Pesticide Resi-due Analytical Laboratory, Hódmezővásárhely

Hódmezovásárhely Yes

Hungary HU Food Chain Safety Centre Nonprofit Ltd. Pesticide Residue Analytical Laboratory, Miskolc

Miskolc Yes

Hungary HU Food Chain Safety Centre Non-profit Ltd., Pesticide Resi-due Analytical Laboratory, Szolnok

Szolnok Yes

Hungary HU National Food Chain Safety Office, Directorate of Plant Protection, Soil Conservation and Agri-environment - Pesticide Analytical Laboratory, Velence

Velence x Yes

Hungary HU Wessling Hungary Ltd. Food Testing Laboratory Budapest Yes

Ireland IE PCL, Backweston Lab Complex Co. Kildare x Yes

Italy IT APPA Bolzano Bolzano Yes

Italy IT ARPA Puglia Bari Yes

Italy IT ARPAE Ferrara Laboratorio Tema Ferrara Yes

Italy IT ARPAV Verona Verona Yes

Italy IT Contaminanti Ambientali Perugia Yes

Italy IT Istituto Superiore di Sanità Rome x No

Italy IT Istituto Zooprofilattico Sperimentale Abruzzo e Molise Teramo Yes

Italy IT IZS Sardegna - Lab Chimica Ambientale e Tossicologia Sassari Yes

Italy IT IZS Sicilia - Pesticide Lab Palermo Yes

Italy IT USL Toscana centro - Lab. Sani Firenze Yes

Italy IT; MT Istituto Zooprofilattico Sperimentale Lombardia ed Emilia Romagna

Brescia Yes

Italy RO IZSLT Roma Yes

Latvia LV Research Institute BIOR Riga x Yes

Lithuania LT NMVRVI Vilnius x Yes

Luxembourg LU LNS-ALI Dudelange x Yes

Norway NO NIBIO, Biotechnology and Plant Health, Pesticides and Natural Products Chemistry

Aas Yes

Poland PL IPP-NRI, Bialystok Bialystok Yes

Poland PL Wojewódzka Stacja Sanitarno-Epidemiologiczna w Opolu Opole Yes

Poland PL WSSE w Warszawie Warszawa x Yes

Poland PO J.S. Hamilton Poland S.A. Gdynia Yes

Poland PO UO-Technologia Grójec Yes

Portugal PT Laboratório Regional de Veterinária e Segurança Alimen-tar

Funchal Madeira Island

x Yes


Appendix 1-a (cont.): participating labs of EU and EFTA member states

Appendix 1. List of Laboratories Registered to Participate in the EUPT-SRM13

A-3

Part

iciP

atio

n

a1Country (Location)


SRMReported

results

Slovakia SK Veterinary and Food Institute in Bratislava Bratislava x Yes

Slovenija SI National Laboratory for Health, Environment and Food - Maribor (location Ljubljana)

Ljubljana Yes

Slovenija SI NLZOH-Maribor Maribor x Yes

Spain ES AINIA PATERNA, VALENCIA Yes

Spain ES Analytica Alimentaria Almeria Yes

Spain ES CNA (AECOSAN) Majadahonda (Ma-drid)

x Yes

Spain ES CNTA San Adrián (Navarra) Yes

Spain ES DIRECCION TERRITORIAL COMERCIO Valencia No

Spain ES EUROFINS SICA AGRIQ, S.L. VÍCAR (ALMERIA) Yes

Spain ES Lab Agroalim. de Extremadura Cáceres Yes

Spain ES Lab Agroamb Zaragoza Zaragoza Yes

Spain ES Lab. Agroalimentario y de Sani El Palmar-Murcia No

Spain ES Laboratori Agència de Salut Pública de Barcelona Barcelona Yes

Spain ES Laboratorio Agrario Abegondo. A Coruña No

Spain ES Laboratorio Agrario Regional, Burgos Yes

Spain ES Laboratorio Arbitral Agroalimentario Madrid x Yes

Spain ES Laboratorio SOIVRE Tenerife Santa Cruz de Tener-ife. Canay Island

Yes

Spain ES LABORATORIOS ECOSUR, S.A. Lorquí (Murcia) Yes

Spain ES LPSVJAEN Mengibar (Jaén) Yes

Spain ES; MT LAGV Burjassot-Valencia Yes

Sweden SE Eurofins Food&Feed Sweden AB Lidkoping Yes

Sweden SE Livsmedelsverket, Dep of Chemi Uppsala x Yes

Switzerland CH Kantonales Labor Zürich Zurich Yes

Switzerland CH Kantonales Labor, Gesundheitsdepartement Basel-Stadt Basel Yes

Switzerland CH LABORATORIUM DER URKANTONE BRUNNEN Yes

The Netherlands

AL; BE; NL

Eurofins Lab Zeeuws-Vlaanderen Graauw Yes

The Netherlands

BE Dr. A. Verwey B.V. Rotterdam Yes

The Netherlands

BE Groen Agro Control Delfgauw Yes

The Netherlands

BE Nofalab B.V. Schiedam Yes

The Netherlands

NL NVWA - NRL for Pesticide Residues in Food and Feed Wageningen x Yes

The Netherlands

NL RIKILT - Wageningen University Wageningen Yes

United Kingdom

UK; MT Fera Science Ltd York x Yes

United Kingdom

UK Concept Life Sciences Ltd Bar Hill Yes

United Kingdom

UK Eurofins Food Testing UK Wolverhampton Yes


Appendix 1-a (cont.): participating labs of EU and EFTA member states


A-4

Appendix 1-b: Participating labs from EU candidate countries and third countries

Country Institution City Reported results

Belarus Food testing laboratory/BelGIM Minsk Yes

Brazil LANAGRO/MG Pedro Leopoldo Yes

Costa Rica LABORATORIO DE ANÁLISIS DE RESIDUOS DE AGROQUÍMI-COS

San José Yes

Peru Unidad del Centro de Control de Insumos y Residuos Tóxicos - SENASA

Lima Yes

Serbia GZZJZ Belgrade Belgrade Yes

Serbia SP LABORATORIJA A.D. BECEJ Yes

Singapore Agri-Food and Veterinary Authority Veterinary Public Health Laboratory Pesticide Residue Section

Singapore Yes

Thailand Central Laboratory Bangkok Yes

Appendix 2. Shipment Evaluation

A-5

A2

Ship

men

t evA

luAt

ion

Appendix 2 Shipment Evaluation

Compilation of shipment duration

1 day 106 labs (81 %)

2 days 14 labs (11 %)

3 days: 7 labs (5 %): 3× IT, ES, PT, USA, AU

> 4 days: 5 labs (4 %): SR, TH, CR, BR, PE

A-6


Appendix 3 Data of Homogeneity Test

Glyphosate Haloxyfop Mepiquat-Cl

Sample No. Portion 1 [mg/kg]

Portion 2 [mg/kg] Sample No. Portion 1

[mg/kg]Portion 2 [mg/kg] Sample No. Portion 1

[mg/kg]Portion 2 [mg/kg]

No. 024 0.840 0.938 No. 024 0.017 0.017 No. 024 0.121 0.136

No. 036 0.923 0.973 No. 036 0.016 0.018 No. 036 0.130 0.135

No. 047 1.017 0.973 No. 047 0.016 0.015 No. 047 0.131 0.124

No. 066 0.885 0.891 No. 066 0.017 0.016 No. 066 0.115 0.128

No. 077 0.914 0.999 No. 077 0.017 0.017 No. 077 0.128 0.134

No. 090 0.866 0.936 No. 090 0.016 0.016 No. 090 0.125 0.132

No. 110 0.842 0.814 No. 110 0.017 0.016 No. 110 0.105 0.113

No. 122 0.825 1.029 No. 122 0.016 0.017 No. 122 0.121 0.125

No. 142 0.969 0.938 No. 142 0.016 0.015 No. 142 0.132 0.128

No. 167 0.922 0.976 No. 167 0.016 0.016 No. 167 0.125 0.141mean / AV* 0.924 / 0.903 mean / AV* 0.016 / 0.017 mean / AV* 0.126 / 0.124

COMPULSORY COMPOUNDSBromide ion Cyromazine Fluazifop

Sample No. Portion 1 [mg/kg]

Portion 2 [mg/kg] Sample No. Portion 1

[mg/kg]Portion 2 [mg/kg] Sample No. Portion 1

[mg/kg]Portion 2 [mg/kg]

No. 024 14.2 15.3 No. 024 0.098 0.116 No. 024 0.053 0.050

No. 036 14.3 16.5 No. 036 0.112 0.121 No. 036 0.050 0.051

No. 047 14.8 14.0 No. 047 0.113 0.106 No. 047 0.045 0.048

No. 066 15.9 14.6 No. 066 0.099 0.109 No. 066 0.054 0.049

No. 077 14.4 14.9 No. 077 0.108 0.108 No. 077 0.052 0.053

No. 090 15.1 15.7 No. 090 0.105 0.108 No. 090 0.050 0.047

No. 110 12.2 13.0 No. 110 0.101 0.094 No. 110 0.048 0.048

No. 122 13.7 15.3 No. 122 0.100 0.104 No. 122 0.049 0.051

No. 142 14.2 13.6 No. 142 0.113 0.106 No. 142 0.049 0.047

No. 167 13.9 16.8 No. 167 0.105 0.116 No. 167 0.049 0.048mean / AV* 14.6 / 15.4 mean / AV* 0.107 / 0.097 mean / AV* 0.049 / 0.049

* mean / AV = Average value of the homogeneity test data [mg/kg] / Assigned value of PT [mg/kg] derived from the population of EU-/EFTA-Laboratories

Appendix 3. Data of Homogeneity Test

A-7

Ho

mo

gen

eity

A3

N-Acetyl-Glyphosate Perchlorate Phosphonic acid QuizalofopSample

No.Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

No. 024 0.696 0.769 No. 024 0.099 0.109 No. 024 1.874 2.082 No. 024 0.061 0.061

No. 036 0.832 0.880 No. 036 0.104 0.117 No. 036 2.161 2.197 No. 036 0.056 0.062

No. 047 0.772 0.817 No. 047 0.108 0.100 No. 047 2.079 2.025 No. 047 0.057 0.056

No. 066 0.725 0.792 No. 066 0.103 0.106 No. 066 1.931 2.011 No. 066 0.063 0.060

No. 077 0.739 0.821 No. 077 0.096 0.111 No. 077 1.902 2.094 No. 077 0.062 0.061

No. 090 0.739 0.750 No. 090 0.104 0.106 No. 090 1.947 2.055 No. 090 0.060 0.054

No. 110 0.654 0.633 No. 110 0.095 0.092 No. 110 1.774 1.668 No. 110 0.056 0.057

No. 122 0.666 0.779 No. 122 0.100 0.100 No. 122 1.866 2.013 No. 122 0.056 0.059

No. 142 0.794 0.762 No. 142 0.110 0.104 No. 142 2.086 2.011 No. 142 0.059 0.055

No. 167 0.716 0.835 No. 167 0.095 0.106 No. 167 1.882 2.209 No. 167 0.057 0.055mean / AV* 0.759 / 0.835 mean / AV* 0.103 / 0.100 mean / AV* 1.99 / 1.86 mean / AV* 0.058 / 0.052

OPTIONAL COMPOUNDS2,4-DB Diquat Glufosinate MPP

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

No. 024 0.187 0.192 No. 024 1.59 1.24 No. 024 0.195 0.211 No. 024 0.164 0.189

No. 036 0.181 0.187 No. 036 1.52 1.64 No. 036 0.211 0.255 No. 036 0.187 0.197

No. 047 0.163 0.167 No. 047 1.29 1.35 No. 047 0.181 0.192 No. 047 0.179 0.178

No. 066 0.194 0.164 No. 066 1.46 1.46 No. 066 0.212 0.202 No. 066 0.171 0.177

No. 077 0.183 0.185 No. 077 1.42 1.61 No. 077 0.216 0.174 No. 077 0.172 0.188

No. 090 0.179 0.169 No. 090 1.39 1.41 No. 090 0.213 0.207 No. 090 0.174 0.179

No. 110 0.172 0.179 No. 110 1.31 1.44 No. 110 0.160 0.167 No. 110 0.155 0.151

No. 122 0.173 0.184 No. 122 1.67 1.57 No. 122 0.149 0.180 No. 122 0.157 0.175

No. 142 0.166 0.180 No. 142 1.47 1.29 No. 142 0.213 0.184 No. 142 0.179 0.173

No. 167 0.165 0.176 No. 167 1.52 1.49 No. 167 0.182 0.237 No. 167 0.171 0.192mean / AV* 0.177 / 0.183 mean / AV* 1.46 / 1.70 ‡ mean / AV* 0.197 / 0.192 mean / AV* 0.489 / 0.188

* mean / AV = Average value of the homogeneity test data [mg/kg] / Assigned value of PT [mg/kg] derived from the population of EU-/EFTA-Laboratories

‡ : statistically uncertain

OPTIONAL COMPOUND (PHOSPHINE)Phsophine (Test Item) Phosphine (PH3-Tube)

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

Sample No.

Portion 1 [mg/kg]

Portion 2 [mg/kg]

No. 001 0.187 0.189 No. 001 0.068 0.082

No. 006 0.170 0.191 No. 005 0.059 0.068

No. 013 0.178 0.185 No. 008 0.077 0.060

No. 016 0.175 0.192 No. 011 0.079 0.064

No. 031 0.167 0.183 No. 017 0.064 0.078

No. 100 0.184 0.180 No. 021 0.063 0.067

No. 114 0.177 0.197 No. 026 0.073 0.059

No. 140 0.170 0.185 No. 041 0.057 0.060

No. 154 0.176 0.192 No. 048 0.062 0.069

No. 172 0.186 0.191 No. 051 0.073 0.076mean / AV* 0.183 / – mean / AV* 0.068 / –


A-8

* RSD = relative standard diviation

Appendix 4 Data of Stability Test

COMPULSORY COMPOUNDSBormide Ion Cyromazine

AV [mg/kg] 15.4 AV [mg/kg] 0.097

Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018

Sample [mg/kg] [mg/kg] [mg/kg] Sample [mg/kg] [mg/kg] [mg/kg]

No. 077 14.4 14.9 13.3 13.8 14.3 13.9 No. 077 0.108 0.108 0.099 0.100 0.116 0.108

No. 110 12.2 13.0 13.8 14.0 14.1 13.8 No. 110 0.101 0.094 0.108 0.104 0.109 0.108

No. 142 14.2 13.6 14.0 15.5 14.6 13.9 No. 142 0.113 0.106 0.103 0.113 0.109 0.114

Mean [mg/kg] 13.73 14.05 14.11 Mean [mg/kg] 0.105 0.105 0.111

RSD* [%] 7.5 % 4.3 % 0.9 % RSD* [%] 6.2 % 4.2 % 1.5 %

Diviation [%] (ref. 1st Anaylsis) — 2.4 % 2.8 % — -0.4 % 5.3 %

Fluazifop Glyphosate

AV [mg/kg] 0.049 AV [mg/kg] 0.903

Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018


No. 077 0.052 0.053 0.051 0.046 0.048 0.051 No. 077 0.914 0.999 0.938 0.942 0.998 0.909

No. 110 0.048 0.048 0.050 0.051 0.052 0.047 No. 110 0.842 0.814 1.017 0.905 0.919 0.819

No. 142 0.049 0.047 0.051 0.050 0.047 0.047 No. 142 0.969 0.938 0.951 1.030 0.922 1.031


RSD* [%] 5.5 % 2.6 % 3.0 % RSD* [%] 8.0 % 2.7 % 6.1 %

Diviation [%] (ref. 1st Anaylsis) — 0.4 % -1.7 % — 5.6 % 2.2 %

Haloxyfop Mepiquat-Cl

AV [mg/kg] 0.017 AV [mg/kg] 0.124

Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018


No. 077 0.017 0.017 0.016 0.019 0.018 0.015 No. 077 0.128 0.134 0.121 0.123 0.139 0.128

No. 110 0.017 0.016 0.015 0.016 0.017 0.018 No. 110 0.105 0.113 0.140 0.128 0.123 0.135

No. 142 0.016 0.015 0.016 0.015 0.019 0.017 No. 142 0.132 0.128 0.126 0.131 0.129 0.133


RSD* [%] 3.7 % 6.6 % 4.4 % RSD* [%] 10.0 % 4.7 % 1.7 %

Diviation [%] (ref. 1st Anaylsis) — 0.1 % 7.1 % — 3.8 % 6.2 %

/ Compulsory Compounds

Appendix 4. Data of Stability Test

A-9

Sta

bili

ty

a4

Phosphonic acid Quizalofop

AV [mg/kg] 1.86 AV [mg/kg] 0.052

Date 03.05.2018 22.05.2018 18.06.2018 Date 25.04.2018 17.05.2018 07.06.2018


No. 077 1.90 2.09 1.84 1.94 2.09 1.94 No. 077 0.062 0.061 0.064 0.060 0.053 0.057

No. 110 1.77 1.67 2.01 1.97 1.94 1.81 No. 110 0.056 0.057 0.057 0.057 0.056 0.063

No. 142 2.09 2.01 1.90 2.09 1.86 1.99 No. 142 0.059 0.055 0.056 0.057 0.059 0.058


RSD* [%] 9.2 % 3.1 % 3.6 % RSD* [%] 4.7 % 5.4 % 4.1 %

Diviation [%] (ref. 1st Anaylsis) — 1.9 % 0.9 % — 0.3 % -1.2 %

* RSD = relative standard diviation; ‡ : statistically uncertain

OPTIONAL COMPOUNDS2,4-DB Diquat

AV [mg/kg] 0.183 AV [mg/kg] 1.70 ‡

Date 25.04.2018 17.05.2018 07.06.2018 Date 03.05.2018 22.05.2018 18.06.2018


No. 077 0.181 0.187 0.188 0.169 0.157 0.170 No. 077 1.42 1.61 1.24 1.45 1.63 1.23

No. 110 0.172 0.179 0.190 0.184 0.161 0.175 No. 110 1.31 1.44 1.43 1.27 1.48 1.45

No. 142 0.166 0.180 0.184 0.182 0.165 0.162 No. 142 1.47 1.29 1.42 1.35 1.34 1.40


RSD* [%] 3.3 % 2.3 % 1.6 % RSD* [%] 5.7 % 1.5 % 3.5 %

Diviation [%] (ref. 1st Anaylsis) — 3.1 % -7.0 % — -4.5 % -0.1 %

Glufosinate MPP

AV [mg/kg] 0.192 AV [mg/kg] 0.188

Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018


No. 077 0.216 0.174 0.192 0.201 0.202 0.218 No. 077 0.172 0.188 0.163 0.180 0.175 0.171

No. 110 0.160 0.167 0.166 0.174 0.175 0.159 No. 110 0.155 0.151 0.171 0.174 0.164 0.154

No. 142 0.213 0.184 0.191 0.176 0.149 0.211 No. 142 0.179 0.173 0.172 0.185 0.155 0.172


RSD* [%] 10.4 % 7.2 % 11.9 % RSD* [%] 8.7 % 2.2 % 4.3 %

Diviation [%] (ref. 1st Anaylsis) — -1.3 % 0.0 % — 2.7 % -2.6 %

N-Acetyl-Glyphosate Perchlorate

AV [mg/kg] 0.835 AV [mg/kg] 0.100

Date 03.05.2018 22.05.2018 18.06.2018 Date 03.05.2018 22.05.2018 18.06.2018


No. 077 0.739 0.821 0.705 0.798 0.823 0.800 No. 077 0.096 0.111 0.094 0.097 0.109 0.105

No. 110 0.654 0.633 0.773 0.771 0.735 0.659 No. 110 0.095 0.092 0.106 0.100 0.109 0.105

No. 142 0.794 0.762 0.753 0.840 0.648 0.785 No. 142 0.110 0.104 0.101 0.107 0.109 0.110


RSD* [%] 10.6 % 2.9 % 8.3 % RSD* [%] 7.0 % 4.8 % 1.3 %

Diviation [%] (ref. 1st Anaylsis) — 5.4 % 1.1 % — -0.4 % 6.5 %

Appendix 4 (cont.): Data of Stability Test / Optional Compounds


A-10

* RSD = relative standard diviation

OPTIONAL COMPOUNDS (PHOSPHINE)Phosphine (Test Item) Phosphine (PH3-Tube)

AV [mg/kg] – AV [mg/kg] –

Date 20.06.2018 19.07.2018 24.09.2018 Date 28.05.2018 19.06.2018 18.07.2018


No. 006 0.170 0.191 0.147 0.156 0.194 0.182 No. 005 0.059 0.068 0.073 0.065 0.075 0.076

No. 016 0.175 0.192 0.149 0.150 0.184 0.189 No. 017 0.064 0.078 0.064 0.067 0.090 0.083

No. 140 0.170 0.185 0.142 0.152 0.194 0.186 No. 026 0.073 0.059 0.075 0.072 0.082 0.078


RSD* [%] 1.69 % 1.58 % 0.90 % RSD* [%] 5.61 % 6.11 % 6.73 %

Diviation [%] (ref. 1st Anaylsis)

— -17.29 % 4.25 % Diviation [%] (ref. 1st Anaylsis) — 3.8 % 20.0 %

Appendix 4 (cont.): Data of Stability Test / Optional Compounds

Appendix 5. Histograms and kernel Density Estimates of z-score Distributions

A-11

A5

His

tog

rAm

m-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5

02468

10121416182022242628

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468

10121416182022242628

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468

1012141618202224

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 502468

1012141618202224

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

14

16

18

20

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

14

16

Appendix 5 Histograms and kernel Density Estimates of z-score DistributionsHistograms and kernel Density Estimates of z-score* Distributions(Results from EU and EFTA Laboratories only)

Mepiquate-Cl (AV derived from entire population)

* Cut-off at z-score = 5;

Haloxyfop (AV derived from entire population)

Range of z-scores

Fluazifop (AV derived from entire population)

Glyphosate (AV derived from entire population)

Cyromazine (AV derived from entire population)

Compulsory Compounds

Bromide Ion (AV derived from entire population)

|z-score| ≤ 2 acceptable2 < |z-score| < 3 questionable

|z-score| ≥ 3 unacceptable







Coun

t of z

-sco

res

Coun

t of z

-sco

res

Range of z-scores Range of z-scores

Coun

t of z

-sco

res

Coun

t of z

-sco

res










Coun

t of z

-sco

res

Coun

t of z

-sco

res

Coun

t of z

-sco

res

Coun

t of z

-sco

res



EUPT-SRM11 | 2016 (Spinach Homogenate)

A-12

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

14

16

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

14

16

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

14

16

18

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

-4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 50

2

4

6

8

10

12

* Cut-off at z-score = 5;

Phosphonic acid (AV derived from entire population)

Perchlorate (AV # derived from entire population)

Quizalofop (AV # derived from entire population)

Range of z-scores

MPP (AV derived from entire population)

N-Acetyl-Glyphosate (AV derived from entire population)

Glufosinate (AV derived from entire population)

Appendix 5 (cont.) Histograms and kernel Density Estimates of z-score* Distributions(Results from EU and EFTA Laboratories only)

* Cut-off at z-score = 5# excluding diquat and phosphine due to high uncertainty of their assigned values

Optional Compounds #

2,4-DB (AV derived from entire population)





Coun

t of z

-sco

res

Coun

t of z

-sco

res










Coun

t of z

-sco

res

Coun

t of z

-sco

res

Coun

t of z

-sco

res

Coun

t of z

-sco

res





Coun

t of z

-sco

res

Range of z-scores

Appendix 6. Graphic Presentation of z-Scores

A-13

A6

z-sc

ore

dis

trib

uti

on

-5-4-3-2-1012345

65

83

*74

102

85

34

105

33

98

112

15

*78

91

*79

*12

*30

55

92

93

56

63

*68

69

67

72

11

21

6

10

14

26

46

2

*54

45

52

*100

*8

*22

37

*20

89

88

82

50

*51

27

*13

31

94

*4

25

16

111

62

*19

1

*49

104

*29

97

48

App

endi

x 6

Gra

phic

Pre

sent

atio

n of

z-S

core

s: C

ompu

lsor

y Co

mpo

unds

Brom

ide

Ion

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le56

labs

90 %

ques

tiona

ble

2 la

bs3

%un

acce

ptab

le4

labs

6 %

fals

e ne

gativ

e1

lab

Ass

igne

d va

lue

=15

.4 m

g/kg

CV

* =

24.0

%M

RRL

=2.

0 m

g/kg

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-14

-5-4-3-2-1012345

2

88

67

35

62

*78

10

*74

*49

*76

16

65

31

42

104

*22

*36

48

*29

89

3

27

*77

98

*32

17

26

37

105

72

96

87

33

*54

*79

69

82

*51

50

71

15

*4

*12

53

*20

52

101

11

97

63

*57

83

34

46

6

91

55

*8

93

14

*7

*30

92

*61

86

60

25

56

84

112

*24

85

*68

109

45

73

*13

106

*19

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-Sc

ores

: Com

puls

ory

Com

poun

ds

Cyro

maz

ine

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le65

labs

82 %

ques

tiona

ble

8 la

bs10

%un

acce

ptab

le6

labs

8 %

fals

e ne

gativ

e1

lab

Ass

igne

d va

lue

=0.

097

mg/

kgC

V*

=23

.5 %

MRR

L =

0.01

mg/

kg

5.15.5

34.844.7

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-15

A6

z-sc

ore

dis

trib

uti

on

-5-4-3-2-1012345

90

10

45

101

104

*76

26

*49

*7

67

35

*13

42

85

53

92

*22

105

62

*20

17

*68

72

*74

*54

87

109

*32

27

3

*8

34

46

69

83

50

*5

21

88

97

38

6

*30

31

*100

*36

*79

60

89

71

2

*12

23

25

52

55

*61

63

33

1

48

86

11

65

66

98

*78

93

28

37

91

96

107

112

56

16

*80

15

*24

*19

41

84

14

*4

*29

73

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-Sc

ores

: Com

puls

ory

Com

poun

ds

Flua

zifo

p(A

ssig

ned

val

ue

and

CV

* d

eriv

ed fr

om e

nti

re p

opu

lati

on)

acce

ptab

le83

labs

97 %

ques

tiona

ble

2 la

bs2

%un

acce

ptab

le1

lab

1 %

fals

e ne

gativ

e1

lab

Ass

igne

d va

lue

=0.

049

mg/

kgC

V*

=20

.3 %

MRR

L =

0.01

mg/

kg

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-16

-5-4-3-2-1012345

105

*5

83

110

*74

17

2

26

65

55

104

63

*76

87

48

*36

*78

15

45

64

*49

60

34

71

43

52

93

14

109

97

73

21

69

112

98

58

33

*29

72

86

46

56

1

*8

*4

106

107

89

6

96

31

70

92

*20

*51

39

*61

10

*24

91

23

27

*32

101

*12

*30

*22

*13

40

67

88

11

16

41

*79

*54

*19

35

37

50

44

*80

103

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-Sc

ores

: Com

puls

ory

Com

poun

ds

Gly

phos

ate

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le78

labs

94 %

ques

tiona

ble

2 la

bs2

%un

acce

ptab

le3

labs

4 %

fals

e ne

gativ

e0

lab

Ass

igne

d va

lue

=0.

903

mg/

kgC

V*

=22

.6 %

MRR

L =

0.03

mg/

kg

6.255.8

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-17

A6

z-sc

ore

dis

trib

uti

on

-5-4-3-2-1012345

*68

105

101

27

26

35

62

104

6

60

*13

2

42

*54

69

71

88

92

91

*20

3

*22

*29

*79

89

*8

10

63

*7

*32

1

*4

21

31

34

46

83

72

*76

96

*74

*12

*19

23

33

*61

84

87

*36

11

52

65

93

98

14

15

17

16

25

*49

55

97

*100

50

48

109

45

85

107

112

*24

37

73

41

56

66

86

*5

*78

*80

*30

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-Sc

ores

: Com

puls

ory

Com

poun

ds

Hal

oxyf

op(A

ssig

ned

val

ue

and

CV

* d

eriv

ed fr

om e

nti

re p

opu

lati

on)

acce

ptab

le78

labs

96 %

ques

tiona

ble

2 la

bs2

%un

acce

ptab

le1

lab

1 %

fals

e ne

gativ

e0

lab

Ass

igne

d va

lue

=0.

017

mg/

kgC

V*

=20

.4 %

MRR

L =

0.00

3 m

g/kg

7.6

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-18

-5-4-3-2-1012345

2

66

63

97

83

*76

89

*5

*36

34

*29

111

107

72

46

11

53

96

106

56

88

69

31

67

*78

10

*79

104

42

87

71

6

52

65

99

112

*32

33

*8

14

60

95

*51

*77

109

1

*4

50

25

98

*54

73

15

70

16

38

*80

*22

55

*74

92

23

45

*61

110

21

*57

*20

*30

91

27

37

93

35

*12

48

26

86

*24

*68

85

105

101

*13

*49

*19

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-Sc

ores

: Com

puls

ory

Com

poun

ds

Mep

iqua

t-Cl

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le76

labs

88 %

ques

tiona

ble

2 la

bs2

%un

acce

ptab

le8

labs

9 %

fals

e ne

gativ

e2

labs

Ass

igne

d va

lue

=0.

124

mg/

kgC

V*

=22

.9 %

MRR

L =

0.01

mg/

kg 5.7 17.2 39.0

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-19

A6

z-sc

ore

dis

trib

uti

on

-5-4-3-2-1012345

55

109

101

35

*79

91

*74

26

*32

3

87

98

71

*7

*8

*20

*12

107

*49

72

89

85

2

*76

34

60

88

46

50

*24

63

83

14

105

45

*36

*22

23

*30

52

93

41

33

16

11

1

*19

69

97

112

*13

86

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-S

core

s: O

ptio

nal C

ompo

unds

2,4-

DB

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le48

labs

92 %

ques

tiona

ble

1 la

b2

%un

acce

ptab

le3

labs

6 %

fals

e ne

gativ

e2

labs

Ass

igne

d va

lue

=0.

183

mg/

kgC

V*

=20

.7 %

MRR

L =

0.01

mg/

kg

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)


A-20

-5-4-3-2-1012345

55

89

105

17

92

*79

109

83

14

*78

2

73

*36

26

*76

60

46

67

33

93

35

112

*4

101

*30

*13

*22

98

34

71

52

86

97

41

107

27

37

45

88

15

16

44

62

63

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-S

core

s: O

ptio

nal C

ompo

unds

Glu

fosi

nate

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le37

labs

84 %

ques

tiona

ble

2 la

bs5

%un

acce

ptab

le5

labs

11 %

fals

e ne

gativ

e3

labs

Ass

igne

d va

lue

=0.

192

mg/

kgC

V*

=28

.7 %

MRR

L =

0.02

mg/

kg

(Res

ults

from

EU

and

EFT

A L

abor

ator

ies

only

, * =

NRL

)

17.6


A-21

A6

z-sc

ore

dis

trib

uti

on

-5-4-3-2-1012345

109

105

83

63

41

89

60

97

27

46

*36

15

67

34

*30

37

92

112

*13

91

52

88

35

101

45

App

endi

x 6

(con

t.)

Gra

phic

Pre

sent

atio

n of

z-S

core

s: O

ptio

nal C

ompo

unds

MPP

(Ass

ign

ed v

alu

e an

d C

V*

der

ived

from

en

tire

pop

ula

tion

)

acce

ptab

le20

labs

80 %

ques

tiona

ble

2 la

bs8

%un

acce

ptab

le3

labs

12 %

fals

e ne

gativ

e1

lab

Ass

igne

d va

lue

=0.

188

mg/

kgC

V*

=18

.9 %

MRR

L =

0.02

mg/

kg

9.1

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A-23

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A-26

Appendix 7 (cont.) Possible Reasons for Poor Performance (ordered by z-scores)

A: Technical problems/diffculties with measurement instrumentation

B: Procedure not properly conducted / Error during sample preparationC: Matrix effect not properly compensatedD: Lack of experienceE: Error in concentration of analytical standard / calibration stockF: Error in the evaluation/interpretation of measurement dataG: Use of inappropriate procedureH: Reporting limit higher than the assigned value

I: Sample weight too small, homogeneity not waranteedJ: Transcription error / Adminitrative fault

K: Result not corrected for low recoveryL: Inappropriate calibration

M: Detection signals strongly interfered by matrix components/Strong chromatographicinterferences

N: Misunderstanding of the definition of the analyteO: ContaminationP: Sample amount not sufficient for quantitative investigationQ: Error in the conversion factorU: Undefined

Bromide ion Assigned value: 15.4 mg/kg

LabCode z-Score Source of error localized? Reason / Remarks

65 -3.5 (FN)

No Our conclution is that this method ""EURL (CRL) Single Residue Method Ver.1, 2009 for Bromide ion"" is not suitable analysis for this type matrices as Soybean Flour. Comment from the Organizer: Looking at the results of the participants employing methods of this type, I must say that the result distribution was remarkably narrow with the median being close to the assigned value. So, the method seems to work, although it is surely not recom-mendable to inject many extracts of this type of commodities (high fat content), to avoid fat accumulation in the injector. We ourselves have used the QuPPe method for the homogeneity and stability tests of bromide. I was personally concerned whether the unsaturated fatty acids would be brominated thus consuming bromide, but a cross-check with the derivatization method resulted in similar results. If you like to study this issue a bit more I would recommend conducting a standard addition experiment and maybe comparing the slope of the standard addition experiment with the slope of the normal calibration curve (in solvent).

B?, G?

83 -3.2 Yes no experience at all with analysis of bromide using LC-MS/MS; not appropriate ex-traction procedure (use of only MeOH without hydration)

D, G

74 -2.9 Yes significant matrix effect. We have not much experience with this matrix C, D

29 2.1 No Reason not found. We may consider to attribute the overestimated result to the procedural standard calibration that we applied; there is the possibility of increased values due to the inherent correction with recovery of this kind of calibration

L?, U

97 3.3 No The samples blank (042) and SRM sample (130) have been analyzed in the same sequence including a reference sample containing 10 mg/kg bromide ion. In the SRM-blank sample (042) 10 mg/kg bromide are detected. While the detected concentration in the SRM sample (bottle 130) is 27.9 mg/kg, this calculated using a slope obtained by standard addition method on the blank 042 sample and undi-luted samples measurements. The extracts are analyzed both undiluted and 5 times diluted. The results of the 5 times diluted extract have been calculated using a slope with a result of 18.4 mg/kg. The peak of the bromide ion does not show a good shape and the measured amounts in the extract are outside the calibration range. Because the results of the 5 times diluted extract are outside the calibration range and the poor peak shape of bromide, the results of the undiluted measurements have been reported. The used method are optimized and validated for fresh product. The reason for poor result is not clear. Further investigation for dried product is needed.

U

Appendix 7 Possible Reasons Reported for Poor Performance (ordered by z-scores)







Appendix 7. Possible Reasons Reported for Poor Performance

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Cyromazine Assigned value: 0.097 mg/kg


2 -3.6 (FN)

Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.

B, G

88 -2.9 Yes "we analyzed cyromazine with two methods in our lab; the QuEChERS method and the QuPPe method. We detected 0,09 mg/kg cyromazine with the QuEPP method and 0,026 mg/kg cyromazine with the QuEChERS method. Only the QuEChERS method is validated for cyromazine and we have no experience in the analysis of cyromazine with QuPPe. For these reasons we trusted the results of the QuEChERS method more than the results of the QuEPP method. Because of the results of the EUPT-SRM13 we will validate the QuPPe method for cyromazine and use the QuEChERS method only for screening."

D, G

67 -2.4 Yes Matrix effect (result from the analysis with the Sweet-Method which usually works well, even for difficult matrix, but obviousely not for soy flour in this PT. Using QuPPe and a HILIC column the result was 0.0094 mg/kg but with high Ionensuppression of approx. 50%.

C

35 -2.3 Yes on classical vegetables, we’ve not problems with cyromazine analysed by Quechers methodology. But we have no experience with soybean flour. Low recovery can be explained by a matrix effect and difficulties on the integration of the cyromazine peak. Quppe as recommended by EURL with specific chromatographic conditions should be better.

C, D

Bromide ion Assigned value: 15.4 mg/kg


48 4.5 Yes wir haben unsere Bromid-Analyse in dem Soja-Mehl des SRM13 noch einmal näher untersucht. Wir verwenden die Methode DIN EN 13191-2 (2000-10) mit GC-ECD-Detektion. Wir verwenden sie für Gemüse, hauptsächlich Salat und bisher schien die Methode sehr robust zu sein - wir haben bisher alle Bromid-Ringversuche bestanden. Ein Problem ist die geringe vorgeschriebene Einwaagemenge für trockene Proben. Da die Konzentration an Bromid im Sojamehl ebenfalls recht niedrig war, mussten wir knapp an der Bestimmungsgrenze messen. Wir haben die Analyse des Ringver-suchs wiederholt, parallel auch einen alten Ringversuch in Brokkoli. Das Ergebnis der Wiederholung in Sojamehl war zwar etwas niedriger als vorher, aber immer noch zu hoch, während die Konzentration in Brokkoli mit dem Referenzwert übereinstimmte. Wir ziehen daraus den Schluss, dass unsere Analysenmethode für das Sojamehl (und vermutlich andere trockene Proben) nicht geeignet ist. Wir wollten aber ohnehin die Bromid-Bestimmung auf die QuPPe-Methode und LC-MS/MS-Detektion umstellen.

C, G


A-28








Cyromazine Assigned value: 0.097 mg/kg


62 -2.2 Yes The recovery obtained in the spiked sample of the blank material was 67 %. It com-plains with the acceptance criteria for recovery in routinary analysis (60-140%), so recovery factor was not applied to correct sample concentration. The low recovery obtained would explain the low concentration submitted for ciromazine (0.0446 mg/kg).

K

78 -2.1 (Yes) No experience; The reason for the poor performance is probably due to problems with extraction efficiency (human error or matrix effect). Investigations in progress.

C, D

74 -2.1 Yes significant matrix effect. We have not much experience with this matrix C, D

3rd-122 2.1 Yes "Error calculation, because we used a factor of two during the calculation of the results for these pesticides. The implementation of the analytical method for theses pesticide is in process in our laboratory; but we consider to send our result of these pesticide to SRM13 as an opportunity in order to have a preliminary evaluation of our analytical performance. Currently we don’t include these pesticide on the scope our analytical method for routine analysis. "

D, F

109 2.9 (Yes) It’s probably a standard problem (ordered 7 years ago). A new one will be ordered and a comparison made

E?

45 3.7 Yes Matrix effect (Area of ILIS of cyromazine in the sample extract was half so big as that in the calitration solutions); Einen Pipettierfehler der Lösung des Internen Stand-ards schließe ich aus, da wir alle Internen Standards in einer Dotierlösung haben. Was ich unter den gegebenen Umständen nicht sagen kann ist, ob beim Ansetzen der Lösung ein Pipettierfehler vorgelegen hat. Den Extrakt haben wir zusätzlich verdünnt gemessen. Allerdings habe wir bei der Verdünnung den Internen Standard aufgestockt (Verdünnung mit Blankextrakt dem interner Standard für Aufarbeitung zugesetzt wurde). Hier bei erhalten wir einen Gehalt von 0,081mg/kg. Allerdings ist die Fläche des IS im verd. Extrakt auch etwas niedriger als in den Kalibrierlösungen. Aktuell setzen wir gerade unsere Stamm- und Arbeitslösungen neu an. Es ist geplant die LVU nach Austausch der Lösungen erneut aufzuarbeiten und die Parameter zu bestimmen. Im Zuge der Nachanalyse der LVU werden wir ggf. die Bestimmung auch gegen eine über das Gesamtverfahren aufgearbeitete Kalibrierung durchführen.

E

106 34.8 Yes Transcription error resulting from difficulties of the submission tool J

19 44.7 Yes Concentration of calibration standard not correct (too low) E








A-29


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3rd-118 -3.2 (FN)

Yes Our standard solution was Fluazifop-butyl, not free acid N

45 -2.2 No Reason not found U

Glyphoaste Assigned value: 0.903 mg/kg


105 -2.4 Yes Out of lab routine scope, we don’t have the experience yet. D

5 -2.1 (Yes) Our lab don`t consider the result of glyphosate as poor performance. The reasons are: our 2 analysts have made overall 6 replacates of the sample SRM13, 6 replicates of recovery (addition to blank SRM13). All above mentioned replicates were analysed with two analytical chormatographic columns: ACCLAIM Trinity and Hypercarb. We have made several dilutions to explore dependance between concentration and dilution factor: 4 graphs each has 6 points=> 24 dilutions. Our LC/MS/MS piping is metallic, so we have to passive the piping. We can`t change pipes into plastic, because plastic pipes don`t tolerate pressure very well. It was the first time to analyse soya matrix for us and Quppe method didn`t perform very well. At the moment we don`t use IS, because it is very expensive to buy it just for PT. If we start analyse samples then we consider to buy it. Perhaps IS facilitates the analysis.

A, D

44 4.8 Yes few experience (less than one year), matrix effect and too less sample used for analy-sis. The result reported was from a sample weight of 0.2 g with clean extract. With a sample weight of 0.5 g, the extract was dirty and, therefore, the result (0.821 mg/kg) was not submitted.

C, D, I

80 6.2 Yes Very likely due to matrice - we never analyse such heavy matrice (20% fat). We do quantification with Standard addition for glyphosate, this seems not appropriate for difficult matrices. Our first results using external calibration gave concentrations of 1.25 mg/kg. With our second extern calibration with more calibartion points we got 1.08 mg Glypho-sate/kg. Comment from Organizer: Standard addition may indeed be associated with an error if the function is curved. If the lower part of the curve is still linear you may skip the upper points and just do a one-point standard addition. Otherwise dilution will help you to reach the linear range. If you use isotope labelled standard it should also behave similarly to the native one in terms of non-linearity, so the ratio should be expectedly still close to linear even if you work within a non-linear range.

C, D; L

103 55.8 (Yes) our method is a screening method used only to determinate if glyphosate is more then 0,1 mg/kg we checked our result and we observed we made a mistake with the amount of inter-nal standard but also in this case we have a lower z-score > 3. we think that the only way to solve our problems is use ionic chromatography.

Haloxyfop Assigned value: 0.017 mg/kg


3rd-115 -3.3 (FN)

Yes No IS was used and therefore the matrix effect not properly compensated. After us-ing IS (Bentazon-D7) the result was 0.173 mg/kg.

C

3rd-116 -2.3 Yes For Haloxyfop, we had 2 group of results, in interval from 0,004mg/kg to 0,009mg/kg, and group with 2 results of 0,014mg/kg and 0,015mg/kg. We calculated the average of first group of results without last two and it was a mistake. If we had calculated the average of all results, z-score would have been satisfactory.

F

105 -2.3 Yes Matrix in not within our routine scope. D


A-30








Mepiquat Assigned value: 0.124 mg/kg


2 -3.7 (FN)


B, G

66 -3.7 (FN)

Yes Transcription error under stress caused by technical problem with LC-MS/MS (actually 0.175 mg/kg)

J

63 -3.3 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.

C, G








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2,4-DB Assigned value: 0.183 mg/kg


55 -3.8 (FN)

Yes Transcritption error (actually not analysed), not routinely analysed J

109 -3.8 (FN)

Yes transcriptional error, actually not analysed J

86 3.0 Yes This poor performance was probably due to the use of an old calibration solution. We did not detect this problem as our 2,4-DB recovery was correct. New standard ordered, investigation ongoing.

E

Mepiquat Assigned value: 0.124 mg/kg


97 -3.1 Yew "The sample has been hydrolyzed by adding water to the weighted fraction of sam-ple. After 10 minutes the extraction is started by acidified methanol extraction. The calculations have been checked and it was OK. The normal used method applies for fruits and vegetables. Because of the sample are an dried product an additional step of hydrolyzation has been applied for the analysis of the SRM material. An investigation has been carried out for the hydrolyzation time by adding water to different fractions of the SRM sample and proceeding to the extraction step after 10 min and over two nights. The results are below: - Starting with the extraction after 10 minutes hydrolyzation time: concentration of mepiquat is 0.026 mg/kg. The results of the first and reported results is 0.027 mg/kg and the waiting time was 15 min. - Starting with the extraction after 2 nights hydrolyzation time: concentration of mepiquat is 0.077 mg/kg . The reason for poor results is a non optimal extraction time of the dried product. This will be further investigated.

D, G

83 -3.1 Yes we have never analyzed Mepiquat in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 0,120 mg/kg

C, D, G

105 2.1 Yes Matrix in not in our routine scope. D

49 17.2 Yes conversion factor for mepiquat ion to mepiquate chlorate was incorrect Q

101 2.4 No The result of the repeat is 0.076 mg / kg. This gives a Z-score of -1.56, which satisfies, which satisfies. No deviations in integration, calibration, standards and control sam-ple were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. The original z-score was just above 2. This in combination with the good scores of the reanalysis is the conclusion that the deviation only applies to the sequence in which the ring test was measured.

U

3rd-122 4.7 Yes Error calculation, because we used a factor of two during the calculation of the results for these pesticides. The implementation of the analytical method for theses pesticide is in process in our laboratory; but we consider to send our result of these pesticide to SRM13 as an opportunity in order to have a preliminary evaluation of our analytical performance. Currently we don’t include these pesticide on the scope our analytical method for routine analysis.

D, F

19 39 Yes Concentration of calibration standard not correct (too low) E


A-32








Glufosinate Assigned value: 0.192 mg/kg


55 -3.6 (FN)

Yes Transcritption error (actually not analysed), not routinely analysed J

89 -3.6 (FN)

Yes No experience with this analyte, re-analysed and evaluated: 0.981 mg/kg, z-score = 0.7

D

105 -3.6 (FN)

Yes Out of lab routine scope, we don’t have the experience yet. D

3rd-121 -3.6 (FN)

Yes detected concentration 0.182 mg/kg < RL (0.5 mg/kg), therefore no numerical result reported.

H

17 -2.6 Yes two analysis and two other for recovery were conducted; errors occured during sample preparation and lack of material no repeatation was possible; no information about the recovery was available, and the result was not corrected by the recovery.

B, R, P

44 2.7 Yes few experience (less than one year), matrix effect and too less sample used for analy-sis. The result reported was from a sample weight of 0.2 g with clean extract. With a sample weight of 0.5 g, the extract was dirty and, therefore, the result (0.19 mg/kg) was not submitted.

C, D, I

62 3.7 Yes The recovery obtained in the spiked sample of the blank material was 42 %. It does not complain with the acceptance criteria for recovery in routinary analysis (60-140%), so recovery factor was applied to correct sample concentration. However, we should have demonstrate good reproducibility before apply this recovery factor

K

63 10.6 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.

C, G








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a7MPP Assigned value: 0.188 mg/kg


109 -3.6 (FN)


105 -2.6 Yes Out of lab routine scope, we don’t have the experience yet. D

35 2.5 Yes we have no experience with this compound (not analysed till today in the labora-tory). Analysed to test us. A correction with glyphosate C13 was done but MPP D3 for recovery correction should be better

D, L

101 9.1 No The result of the repeat is 0.268 mg / kg. This gives a Z-score of 1.7, which satisfies. No deviations in integration, calibration, standards and control sample were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. This component is kept in the control card and there are no deviations in the chard. Because the re-analysis is good, this deviation also applies only to the sequence in which it was measured.

U

45 19 Yes bad chromatography (small and wide peak, perhaps column not sufficiently precon-ditioned)

B?, M

N-Acetyl glyphosate Assigned value: 0.835 mg/kg


45 -3.9 (FN)

Yes transcrpition errer (confusing between n-acetyl-glyphosate and n-ycetyl-glufosi-nate); ich muss gestehen, dass ich mir bei dem N-Acetyl-Glyphosat nicht die Abwei-chung zum assigned value angesehen hatte. Wir haben das N-Acetyl-Glyphosat gegen das isotopenmarkierte Glyphosat als Internem Standard ausgewertet. Bei der erneuten Durchsicht der Daten ist mir aufgefallen, dass die Widerfindung für das N-Acetylglyphosat um den Faktor 2 zu hoch ist, während die Wiederfindung für Glyphosat i.O. ist (98%). Die Fläche des Internen Standards ist im LVU-Probenextrakt geringer als in den Kalibrierlösungen, was den Überbefund erklären könnte (für die Kalibrierung dotieren wir den Blank-Extrakt an, keine Kalibrierung über Gesamtver-fahren). Auswertung ohne internen Standard gegen die externe Kalibrierung liefert etwas geringere Werte von ~1,0 mg/kg. Aktuell setzen wir gerade unsere Stamm- und Arbeitslösungen neu an. Es ist geplant die LVU nach Austausch der Lösungen erneut aufzuarbeiten und die Parameter zu bestimmen. Im Zuge der Nachanalyse der LVU werden wir ggf. die Bestimmung auch gegen eine über das Gesamtverfahren aufgearbeitete Kalibrierung durchführen.

J

55 -3.9 (FN)

Yes Transcritption error (actually not analysed) The N acetylglyphosate is not analyzed because the Hypercarb column is too tricky to maintain in routine flow. So we let it for an ionic column and it’s impossible to get it

J

76 -3.9 (FN)

Yes Transcription error. (This was a result submission error. This compound is not part of the laboratory’s scope. It is not a true false negative result, the laboratory does not currently analyse for n-acetyl-glyphosate.)

J

89 -3.9 (FN)

Yes No experience with this analyte D

109 -3.9 (FN)


34 76 Yes Standard used (pure substance) for calculation was probably degradeted (cp. with a new standard resulted to a factor of 25.)

E


A-34








Perchlorate Assigned value: 0.100 mg/kg


2 -3.6 (FN)


B, G

109 -3.6 (FN)


83 -3.1 Yes we have never analyzed perchlorate in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 0,090 mg/kg.

C, D, G

63 -2.7 (Yes) We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.

C, G








A-35


Rea

son

foR

poo

R peR

foRm

an

ce

a7Perchlorate Assigned value: 0.100 mg/kg


35 -2.1 Yes we have no experience with soybean flour. A correction with fosetyl D15 is done and usually give us good results. Perchlorate O18 for recovery correction should be better.

D, L

26 2.4 Yes Soy matrix little analyzed by the laboratory - essentially water-rich matrix - no ac-creditation on perchlorate; Intégration large sur la 1ère analyse et ajouts dosé trop importants par rapport à la concentration cible. Relance avec ajouts dosé plus faibles (0,2 et 0,4) qui permettent d'obtenir un résultat conforme. Suivi de ce paramètre sur les essais ultérieurs.

D

69 3.7 Yes Precipitation of stock solution (1mg/ml MeOH with 5% FA) stored at -20 °C that was not redisolved at ambient temperature. New stock prepared in 50% MeOH/50% Water with 5% FA. No ppt even stored at low temperature. With new stock: conc. determined at 0,077 mg/kg, corresponding to a z.score of -0.9; Recovery: 77%

E

101 9.5 No The cause was probably the concentration of the blank that was forgotten to take of the result. The result after blank correction is (0.355-0.214) 0.121 mg / kg. This yields a Z score of 0.85. This does meet. The deviation of perchlorate applies, however, only to this sequence. In "regular" samples no blank is included and therefore no blank deduction is possible.

U

Phosphonic acid Assigned value: 1.86 mg/kg


11 -3.9 (FN)

Yes Transcription error resulting from difficulties of the submision tool (actually not analysed at all)

J

97 -3.9 (FN)

Yes The peak of phosphonic acid detected in the sample fulfills the criteria of retention time and MRM ratio, (see the chromatograms 1 and 2). By adding a known amount of phosphonic acid to a second fraction of the sample, by applying the standard addi-tion method, the detected peak splits in to two peaks that are not totally separated. The detected peak of phosphonic acid in the first fraction without addition is consid-ered as false positive and the results are not reported. Because of a poor z-score the extracts analyses performed on the SRM material are repeated with a 20 times extra dilution of the extracts compared to the initial meas-urements performed by the first analyses of the SRM samples. The obtained peaks shape was good and the splitting in the spiked extract was not observed, (see the chromatograms 3 and 4). The reason for poor results is an insufficient chromatography method application. A new method will be developed using a different column with more separation power.

F, G

2 -3.7 Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuEChERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.

B, G


A-36








Phosphonic acid Assigned value: 1.86 mg/kg


83 -3.2 Yes Until now, we have never analyzed Phosphonic acid in cereals or oilseeds. We believe that the unsatisfactory results are due to the fact that we used 5 grams of sample and did not hydrate with water before extraction. After seeing the results in the preliminary report, we repeated the extraction using 2 grams of sample and hydrating with 5 mL of water for 1 hour before extraction. The result obtained now is 2,90 mg/kg.

C, D, G

63 -3.2 Yes We have checked the standars solutions involved in the test, some of them with reference material and after repeating the extractions, we would need more time to perform other extraction methods because we believe that it could be the problem to obtain a correct quantification.

C, G

91 -2.5 Yes Despite the fact, that the isotopically labelled phosphorus acid standard has been used and the prepared spike in the blank matrix has provided a satisfactory value, these measures did not provide effective help in case of the correct determination of phosphonic acid as incurred residues. After re-extraction of sample, when 2.5 g was weighted and soaking time was extended to 30 min (instead of 10 min in original procedure), we obtained the concentration of phosphonic acid 1.871 mg/kg. Considering this fact the soaking time seems to be the key parameter for our originally reported concentration level of phosphonic acid.

G

41 12.1 (Yes) in the same analytical batch we processed the EUPT_SRM12 material and we obtained the acceptable result for this molecule. So we believed that EUPT_SRM13 results was good. Now we are testing our standard pool and single Phosphonic acid solution to verify the retention time and possible degradation of other pesticides in pool to Phosphonic acid.

E?








A-37


Rea

son

foR

poo

R peR

foRm

an

ce

a7Quizalofop Assigned value: 0.052 mg/kg


47 -4 (FN)

Yes The active substance that we analyzed is Quizalofop-ethyl CAS No. 76578. (The analy-sis was carried out by extraction with acetonitrile, cleaning with PSA and evaporation of the extract in a stream of nitrogen. The addition made to the white sample at the level of 0.01 mg / kg gives a correct recovery of 68%.)

U

66 -3.2 (FN)

Yes Transcription error under stress caused by technical problem with LC-MS/MS (actually 0.034 mg/kg)

J

3rd-118 -3.2 (FN)

Yes Our standard solution was Quizalofop-ethyl, not free acid N

76 -2.3 Yes Ne experience and special matrix effect of soybean flour. (Soybean flour is not tested routinely in our laboratory. There was a poor recovery of quizalofop in the lab soybean flour spike (56%) analysed with this PT scheme. This poor recovery is unique to soybean flour and not other cereals analysed by the laboratory. The lab did not correct for recovery. If the lab had corrected for recovery in the spike then the z-score would have been acceptable.)

C, D

26 -2.2 Yes Soy matrix little analyzed by the laboratory - essentially water-rich matrix - no ac-creditation on quizalofop; Sous dosage lors de la 1ère analyse, rendement pris en compte lors du rendu. Relance conforme. Problème ponctuel d'extraction

D

101 -2.2 No The result of the repeat is 0.030 mg / kg. This gives a Z-score of -1.7, which satisfies. No deviations in integration, calibration, standards and control sample were detected. No apparent cause was found for the abnormality. The deviation for MPP is very high. The original z-score was just below -2. This in combination with the good scores of the reanalysis is the conclusion that the deviation only applies to the sequence in which the ring test was measured.

U

112 2.2 Yes the evaluation of this non-conformity showed that the standard used for Quizalofop was 20% too low, presumably due to precipitation. When correcting for this factor, we would have found a value of 0,064 mg/kg, thus well within the acceptable range

U

2 2.4 Yes Although we generally add water in extraction of dry cereal- and cereal based prod-ucts, we did not add water to this ‘dry oil-containing soybean’ PT- sample. After internal investigation it is clear that we should have added water to this matrix-type in order to achieve a good extraction efficiency. We have retested the sample with water addition and would have obtained a good result for the poor performing compounds. Comment from Organizer: For oily seeds and nuts we use a Variant of the QuOil Method, in which we use as extraction solvent ACN containing 5% Wasser. Without the addition of water we have also observed severe losses of certain pesticides with polar groups, that tend to interact with surfaces. For the analytes relevant to the EUPT-SRM13, QuEChERS for dry products (involving addition of 10 mL water) also works well. For acidic pesticides the use of PSA sorbent in dSPE-cleanup is critical of course. In absence of water, interactions of pesticides with PSA are generally stronger and more pesticides are negatively affected than when dSPE cleanup is conducted on QuECh-ERS extracts of fruits and vegetables. The 5% water mentioned above is thus helpful in the cleanup step as well. We intend to soon launch an interalboratory validation round for the abovemen-tioned Variant of the QuOil Method with the focus being on nuts and oily seeds. If you are interested to take part, just tell me.

B, G


A-38








False Positive ResultsAnalyte LabCode Reason / Remarks

Ethephon 41 we determined the pesticide using only one transition and now we are trying to use a second qualifier transition to be compliant to SANTE regulation

G

N-Acetyl glufosinate

45 transcrition errer (confusing between n-acetyl-glyphosate and n-ycetyl-glufosinate) J

AMPA 41 we quantified an interfering peak, so we tried to change the quantifier ion F, M

AMPA 3rd-118 For Glyphosate we use HPLC with post column derivertizer and analysis Glyphosate and AMPA (N-Acetyl-Glyphosate not analysis), we found AMPA in blank. Our LC con-dition had the wrong separation due to dry soybean matrix or N-Acetyl-Glyphosate . We will purchase N-Acetyl-Glyphosate standard and check again. Comment form Organizer: Contamination

C, M, O

Paraquat 3rd-118 Paraquat we use LC-MS, Idenitfication not enough for dry soybeans matrix due to we found paraquat in sample blank cannot separate paraquat with matrix in soybeans Comment form Organizer: Contamination

C, O

A-39

Appendix 8 (cont.) General EUPT Protocol (8th Ed.)

A8

Gen

erA

l Pro

toco

(8th

ed

.)

Appendix 8. General EUPT Protocol (8th Ed.)

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 1

of 1

6

GEN

ERA

L PR

OTO

CO

L fo

r EU

Pro

ficie

ncy

Test

s on

Pes

ticid

e R

esid

ues

in

Foo

d an

d Fe

ed

Intr

oduc

tion

This

pro

toco

l con

tain

s ge

nera

l pro

cedu

res

valid

for

all E

urop

ean

Uni

on P

rofic

ienc

y Te

sts

(EU

PTs)

or

gani

sed

on b

ehal

f of

the

Eur

opea

n C

omm

issi

on,

DG

-SAN

TE1

by t

he f

our

Euro

pean

Uni

on

Ref

eren

ce L

abor

ator

ies

(EU

RLs

) re

spon

sibl

e fo

r pe

stic

ide

resi

dues

in

food

and

fee

d. T

hese

EU

PTs

are

dire

cted

at l

abor

ator

ies

belo

ngin

g to

the

Net

wor

k2 of

Nat

iona

l Ref

eren

ce L

abor

ator

ies

(NR

Ls)

and

Offi

cial

Lab

orat

orie

s (O

fLs)

of t

he E

U M

embe

r St

ates

. OfL

s fro

m E

FTA

coun

tries

and

EU

-Can

dida

te c

ount

ries

are

also

wel

com

e to

par

ticip

ate

in th

e EU

PTs.

OfL

s fro

m T

hird

cou

ntrie

s m

ay b

e pe

rmitt

ed to

par

ticip

ate

on a

cas

e-by

-cas

e ba

sis.

The

follo

win

g fo

ur E

UR

Ls f

or p

estic

ide

resi

dues

wer

e ap

poin

ted

by D

G-S

ANTE

bas

ed o

n re

gula

tion

(EC

) 625

/201

73 :

EU

RL

for F

ruits

and

Veg

etab

les

(EU

RL-

FV),

EU

RL

for C

erea

ls a

nd F

eedi

ngst

uffs

(EU

RL-

CF)

,

EU

RL

for F

ood

of A

nim

al O

rigin

and

Com

mod

ities

with

Hig

h Fa

t Con

tent

(EU

RL-

AO) a

nd

EU

RL

for p

estic

ides

requ

iring

Sin

gle

Res

idue

Met

hods

(EU

RL-

SRM

).

The

aim

of t

hese

EU

PTs

is to

obt

ain

info

rmat

ion

rega

rdin

g th

e qu

ality

, acc

urac

y an

d co

mpa

rabi

lity

of p

estic

ide

resi

due

data

in fo

od a

nd fe

ed re

porte

d to

the

Euro

pean

Uni

on w

ithin

the

fram

ewor

k of

th

e na

tiona

l co

ntro

l pr

ogra

mm

es a

nd t

he

EU m

ultia

nnua

l co

-ord

inat

ed c

ontro

l pr

ogra

mm

e4 . Pa

rtici

patin

g la

bora

torie

s w

ill be

pro

vide

d w

ith a

n as

sess

men

t of t

heir

anal

ytic

al p

erfo

rman

ce th

at

1 DG

-SA

NTE

= E

urop

ean

Com

mis

sion

, Hea

lth a

nd F

ood

Saf

ety

Dire

ctor

ate-

Gen

eral

2 F

or m

ore

info

rmat

ion

abou

t the

EU

RL/

NR

L/O

fL-N

etw

ork

plea

se re

fer t

o th

e E

UR

L-W

eb-p

orta

l und

er:

ht

tp://

ww

w.e

url-p

estic

ides

.eu

3 Reg

ulat

ion

(EU

) 201

7/62

5 of

the

Eur

opea

n P

arlia

men

t and

of t

he C

ounc

il on

offi

cial

con

trols

and

oth

er o

ffici

al a

ctiv

ities

pe

rform

ed to

ens

ure

the

appl

icat

ion

of fo

od a

nd fe

ed la

w, r

ules

on

anim

al h

ealth

and

wel

fare

, pla

nt h

ealth

and

pla

nt

prot

ectio

n pr

oduc

ts..

Pub

lishe

d at

OJ

of th

e E

U L

95 o

f 07.

04.2

017

4 Eur

opea

n C

omm

issi

on P

rofic

ienc

y Te

sts

for P

estic

ide

Res

idue

s in

Fru

its a

nd V

eget

able

s, T

rend

s in

Ana

lytic

al

Che

mis

try, 2

010,

29

(1),

70 –

83.

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 2

of 1

6

they

can

use

to

dem

onst

rate

the

ir an

alyt

ical

per

form

ance

and

com

pare

the

mse

lves

with

oth

er

parti

cipa

ting

labo

rato

ries.

EU

PT-O

rgan

iser

s an

d Sc

ient

ific

Com

mitt

ee

EUPT

s ar

e or

gani

sed

by in

divi

dual

EU

RLs

, or b

y m

ore

than

one

EU

RL,

in jo

int c

olla

bora

tion.

An O

rgan

isin

g Te

am i

s ap

poin

ted

by t

he E

UR

L(s)

in

char

ge.

This

tea

m i

s re

spon

sibl

e fo

r al

l ad

min

istra

tive

and

tech

nica

l m

atte

rs

conc

erni

ng

the

orga

nisa

tion

of

the

PT,

e.g.

th

e PT

-an

noun

cem

ent,

prod

uctio

n of

Tes

t Ite

m a

nd B

lank

Mat

eria

l, th

e un

derta

king

of

hom

ogen

eity

and

st

abilit

y te

sts,

pac

king

and

shi

pmen

t of t

he T

est I

tem

and

Bla

nk M

ater

ial,

hand

ling

and

eval

uatio

n of

the

res

ults

and

met

hod

info

rmat

ion

subm

itted

by

the

parti

cipa

nts

and

the

draf

ting

of t

he

prel

imin

ary

and

final

repo

rts.

To c

ompl

emen

t the

inte

rnal

exp

ertis

e of

the

EUR

Ls, a

gro

up o

f ext

erna

l con

sulta

nts

that

form

the

EUPT

-Sci

entif

ic C

omm

ittee

(EU

PT-S

C)5 h

as b

een

esta

blis

hed

and

appr

oved

by

DG

-SAN

TE. T

he

EUPT

-SC

con

sist

s of

exp

ert

scie

ntis

ts w

ith m

any

year

s of

exp

erie

nce

in P

Ts a

nd/o

r pe

stic

ide

resi

due

anal

ysis

. The

act

ual c

ompo

sitio

n of

the

EUPT

-SC

, the

affi

liatio

n of

eac

h m

embe

r is

show

n on

the

EU

RL-

Web

site

. The

mem

bers

of

the

EUPT

-SC

will

also

be

liste

d in

the

Spe

cific

Pro

toco

l an

d th

e Fi

nal R

epor

t of e

ach

EUPT

.

The

EUPT

-SC

is m

ade

up o

f the

follo

win

g tw

o su

bgro

ups:

a)

An in

depe

nden

t Qua

lity

Con

trol

Gro

up (E

UPT

-QC

G) a

nd

b)

An A

dvis

ory

Gro

up (E

UPT

-AG

).

The

EUPT

-SC

’s r

ole

is t

o he

lp t

he O

rgan

iser

s m

ake

deci

sion

s re

gard

ing

the

EUPT

des

ign:

the

se

lect

ion

of th

e co

mm

odity

, the

sel

ectio

n of

pes

ticid

es to

be

incl

uded

in th

e Ta

rget

Pes

ticid

e Li

st

(see

bel

ow),

the

esta

blis

hmen

t of t

he M

inim

um R

equi

red

Rep

ortin

g Le

vels

(MR

RLs

), th

e st

atis

tical

tre

atm

ent a

nd e

valu

atio

n of

par

ticip

ants

resu

lts (i

n an

onym

ous

form

), an

d th

e dr

aftin

g an

d up

datin

g of

doc

umen

ts s

uch

as th

e G

ener

al a

nd S

peci

fic P

T Pr

otoc

ols

and

the

Fina

l EU

PT-R

epor

ts.

The

EUPT

-QC

G h

as th

e ad

ditio

nal f

unct

ion

of s

uper

visi

ng t

he q

ualit

y of

EU

PTs

and

of a

ssis

ting

the

EUR

Ls in

con

fiden

tial a

spec

ts s

uch

as th

e ch

oice

of

the

pest

icid

es to

be

pres

ent i

n th

e Te

st

Item

and

the

conc

entra

tions

at w

hich

they

sho

uld

be p

rese

nt.

5 Lin

k to

the

List

of c

urre

nt m

embe

rs o

f the

EU

PT

Sci

entif

ic C

omm

ittee

: ht

tp://

ww

w.e

url-p

estic

ides

.eu/

libra

ry/d

ocs/

allc

rl/E

UP

T-S

C.p

df

Appendix 8 General EUPT Protocol (8th Ed.)


A-40


8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 4

of 1

6

NR

Ls a

re r

espo

nsib

le f

or c

heck

ing

whe

ther

all

rele

vant

OfL

s w

ithin

the

ir ne

twor

k ar

e in

clud

ed in

th

e lis

t of

obl

igat

ed la

bora

torie

s an

d w

heth

er t

he c

onta

ct in

form

atio

n an

d co

mm

odity

-sco

pes

are

corr

ect.

OfL

s ar

e fu

rther

mor

e ur

ged

to k

eep

thei

r ow

n pr

ofile

s w

ithin

the

EU

RL-

Dat

aPoo

l up

-to-d

ate,

es

peci

ally

thei

r com

mod

ity a

nd p

estic

ide

scop

es a

nd th

eir c

onta

ct in

form

atio

n.

Labs

tha

t ar

e ob

liged

to

parti

cipa

te in

a g

iven

EU

PT,

and

that

are

not

abl

e to

par

ticip

ate,

mus

t pr

ovid

e th

e re

ason

s fo

r th

eir

non-

parti

cipa

tion

with

out p

reju

dice

of a

ny le

gal a

ctio

n ta

ken

agai

nst

them

for

not p

artic

ipat

ing.

Thi

s al

so a

pplie

s to

any

par

ticip

atin

g la

bora

torie

s th

at th

en fa

il to

rep

ort

resu

lts.

Base

d on

Reg

. (E

C)

625/

2017

, O

fLs

not

payi

ng t

he E

UPT

sam

ple

deliv

ery

fee

will

be i

nitia

lly

war

ned

that

thei

r pa

rtici

patio

n in

sub

sequ

ent E

UPT

s co

uld

be d

enie

d. In

cas

e of

a r

epet

itive

non

-pa

ymen

t, th

e EU

PT o

rgan

iser

s w

ill in

form

the

com

pete

nt a

utho

rity

to ta

ke a

ctio

n.

Con

fiden

tialit

y an

d C

omm

unic

atio

n

The

prop

rieto

r of a

ll EU

PT d

ata

is D

G-S

ANTE

and

as

such

has

acc

ess

to a

ll in

form

atio

n.

For

each

EU

PT,

the

labo

rato

ries

are

give

n a

uniq

ue c

ode

(lab

code

), in

itial

ly o

nly

know

n to

th

emse

lves

and

the

Org

anis

ers.

In th

e fin

al E

UPT

-Rep

ort,

the

nam

es o

f par

ticip

atin

g la

bora

torie

s w

ill no

t be

linke

d to

thei

r lab

orat

ory

code

s. It

sho

uld

be n

oted

, how

ever

, tha

t the

Org

anis

ers,

at t

he

requ

est

by D

G-S

ANTE

, m

ay p

rese

nt t

he E

UPT

-resu

lts o

n a

coun

try-b

y-co

untry

bas

is.

It m

ay

ther

efor

e be

pos

sibl

e th

at a

link

bet

wee

n co

des

and

labo

rato

ries

coul

d be

mad

e, e

spec

ially

for

th

ose

coun

tries

whe

re o

nly

one

labo

rato

ry h

as p

artic

ipat

ed.

Furth

erm

ore,

the

EUR

Ls r

eser

ve th

e rig

ht t

o sh

are

EUPT

res

ults

and

cod

es a

mon

gst

them

selv

es:

for

exam

ple,

for

the

pur

pose

of

eval

uatin

g ov

eral

l lab

or c

ount

ry p

erfo

rman

ce a

s re

ques

ted

by D

G-S

ANTE

.

As la

id d

own

in R

egul

atio

n 62

5/20

17, N

RLs

are

resp

onsi

ble

for s

uppo

rting

and

impr

ovin

g th

eir o

wn

OfL

-Net

wor

k. O

n re

ques

t fro

m t

he N

RLs

, th

e EU

RLs

will

prov

ide

them

with

the

PT-

code

s of

the

pa

rtici

patin

g O

fLs

belo

ngin

g to

the

ir O

fL-N

etw

ork.

Thi

s w

ill al

low

NR

Ls t

o fo

llow

the

par

ticip

atio

n an

d pe

rform

ance

of t

he la

bora

torie

s w

ithin

thei

r net

wor

k.

Com

mun

icat

ion

betw

een

parti

cipa

ting

labo

rato

ries

durin

g th

e te

st o

n m

atte

rs c

once

rnin

g a

PT

exer

cise

is n

ot p

erm

itted

from

the

star

t of t

he P

T ex

erci

se u

ntil

the

dist

ribut

ion

of th

e pr

elim

inar

y re

port.

For

each

EU

PT t

he o

rgan

isin

g EU

RL

prep

ares

a s

peci

fic E

UPT

-Web

site

whe

re a

ll re

leva

nt

docu

men

ts in

thei

r lat

est v

ersi

on a

re li

nked

.

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 3

of 1

6

The

EUPT

-SC

typi

cally

mee

ts o

nce

a ye

ar, a

fter t

he E

UPT

s of

all

four

pes

ticid

e EU

RLs

hav

e be

en

cond

ucte

d, t

o di

scus

s th

e ev

alua

tion

of t

he E

UPT

-resu

lts a

nd t

o co

nsul

t with

the

EU

RLs

in t

heir

deci

sion

mak

ing.

Upc

omin

g EU

PTs

are

also

pla

nned

dur

ing

thes

e m

eetin

gs.

The

EUPT

-Org

anis

ing

Team

and

the

EUPT

-SC

toge

ther

form

the

EUPT

-Pan

el.

The

deci

sion

s of

the

EUPT

-Pan

el w

ill be

doc

umen

ted.

This

pre

sent

EU

PT G

ener

al P

roto

col w

as jo

intly

dra

fted

by th

e EU

PT-S

C a

nd th

e EU

RLs

and

was

ap

prov

ed b

y D

G-S

ANTE

.

EUPT

Par

ticip

ants

With

in th

e Eu

rope

an U

nion

all

NR

Ls o

pera

ting

in th

e sa

me

area

as

the

orga

nisi

ng E

UR

L, a

s w

ell

as a

ll O

fLs

who

se s

cope

ove

rlaps

with

tha

t of

the

EU

PT,

are

lega

lly o

blig

ed t

o pa

rtici

pate

in

EUPT

s. T

he le

gal o

blig

atio

n of

NR

Ls a

nd O

fLs

to p

artic

ipat

e in

EU

PTs

aris

es fr

om:

- Ar

t. 28

of

Reg

. 39

6/20

05/E

C6

(for

all

OfL

s an

alys

ing

for

pest

icid

e re

sidu

es w

ithin

the

fra

mew

ork

of o

ffici

al c

ontro

ls7 o

f foo

d or

feed

)

- Ar

t. 10

1 (1

)(a) o

f Reg

. (EC

) 625

/201

7 (fo

r all

NR

Ls)

The

four

EU

RLs

will

annu

ally

issu

e an

d di

strib

ute,

via

the

EUR

L-w

ebsi

te, a

join

t lis

t of a

ll O

fLs

that

m

ust p

artic

ipat

e in

eac

h of

the

EUPT

s to

be

cond

ucte

d w

ithin

a g

iven

yea

r. Th

e lis

t of o

blig

ed la

bs

will

be u

pdat

ed e

very

yea

r to

take

acc

ount

of a

ny c

hang

es in

the

lab

prof

iles.

Inte

rim u

pdat

es w

ill be

issu

ed to

elim

inat

e an

y po

ssib

le e

rror

s.

6 R

egul

atio

n (E

C) N

o 39

6/20

05, p

ublis

hed

at O

J of

the

EU

L70

of 1

6.03

.200

5, a

s la

st a

men

ded

by R

egul

atio

n 83

9/20

08

publ

ishe

d at

OJ

of th

e E

U L

234

of 3

0.08

.200

8.

7 Offi

cial

con

trols

in th

e se

nse

of R

eg. (

EC

) 625

/201

7. T

his

incl

udes

labs

invo

lved

in c

ontro

ls w

ithin

the

fram

ewor

k of

na

tiona

l and

/or E

U-c

ontro

lled

prog

ram

mes

as

wel

l as

labs

invo

lved

in im

port

cont

rols

acc

ordi

ng to

Reg

ulat

ion

669/

2009

/EC

.

OR

GAN

ISER

S EU

PT-A

G

EUPT

-QC

G

EUPT

-Pan

el

EUPT

-SC


A-41


A8

Gen

erA

l Pro

toco

(8th

ed

.)

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 5

of 1

6

The

offic

ial l

angu

age

used

in a

ll EU

PTs

is E

nglis

h.

Anno

unce

men

t / In

vita

tion

Lette

r

At

leas

t 3

mon

ths

befo

re

the

dist

ribut

ion

of

the

Test

Ite

m

the

EUR

Ls

will

publ

ish

an

Anno

unce

men

t/Inv

itatio

n le

tter

on th

e EU

RL-

web

-por

tal a

nd d

istri

bute

it v

ia e

-mai

l to

the

NR

L/O

fL

mai

ling

list a

vaila

ble

to th

e EU

RLs

. Thi

s le

tter w

ill in

form

abo

ut th

e co

mm

odity

to b

e us

ed a

s Te

st

Item

, as

wel

l as

links

to th

e te

ntat

ive

EUPT

-Tar

get P

estic

ide

List

and

the

tent

ativ

e E

UPT

-Cal

enda

r.

Targ

et P

estic

ide

List

This

list

con

tain

s al

l ana

lyte

s (p

estic

ides

and

met

abol

ites)

to b

e so

ught

, alo

ng w

ith t

he M

inim

um

Req

uire

d R

epor

ting

Leve

ls (

MR

RLs

) va

lid f

or th

e sp

ecifi

c EU

PT. T

he M

RR

Ls a

re ty

pica

lly b

ased

up

on

the

low

est

MR

Ls

foun

d ei

ther

in

R

egul

atio

n 39

6/20

05/E

C

or

Com

mis

sion

D

irect

ive

2006

/125

/EC

(Bab

y Fo

od D

irect

ive)

.

Labs

mus

t exp

ress

thei

r res

ults

as

stat

ed in

the

Targ

et P

estic

ides

Lis

t.

Spec

ific

Prot

ocol

For

each

EU

PT t

he o

rgan

izin

g EU

RL

will

publ

ish

a Sp

ecifi

c Pr

otoc

ol a

t lea

st 2

wee

ks b

efor

e th

e Te

st I

tem

is d

istri

bute

d to

the

par

ticip

atin

g la

bora

torie

s. T

he S

peci

fic P

roto

col w

ill co

ntai

n al

l the

in

form

atio

n pr

evio

usly

inc

lude

d in

the

Inv

itatio

n Le

tter

but

in i

ts f

inal

ver

sion

, in

form

atio

n on

pa

ymen

t an

d de

liver

y, in

stru

ctio

ns o

n ho

w t

o ha

ndle

the

Tes

t Ite

m u

pon

rece

ipt

and

on h

ow t

o su

bmit

resu

lts, a

s w

ell a

s an

y ot

her r

elev

ant i

nfor

mat

ion.

Hom

ogen

eity

of t

he T

est I

tem

The

Test

Ite

m w

ill be

tes

ted

for

hom

ogen

eity

typ

ical

ly b

efor

e di

strib

utio

n to

par

ticip

ants

. Th

e ho

mog

enei

ty t

ests

usu

ally

invo

lve

the

anal

ysis

of

two

repl

icat

e an

alyt

ical

por

tions

, ta

ken

from

at

leas

t ten

rand

omly

cho

sen

units

of t

reat

ed T

est I

tem

. Bot

h, s

ampl

e pr

epar

atio

n an

d m

easu

rem

ents

sh

ould

be

cond

ucte

d in

rand

om o

rder

.

The

hom

ogen

eity

test

dat

a ar

e st

atis

tical

ly e

valu

ated

acc

ordi

ng to

ISO

135

28, A

nnex

B o

r to

the

In

tern

atio

nal H

arm

oniz

ed P

roto

cols

join

tly p

ublis

hed

by IS

O, A

OAC

and

IUPA

C. T

he r

esul

ts o

f all

hom

ogen

eity

test

s ar

e pr

esen

ted

to th

e EU

PT-S

C. I

n sp

ecia

l cas

es, w

here

the

abov

e ho

mog

enei

ty

test

crit

eria

are

not

met

, th

e EU

PT-S

C c

onsi

derin

g al

l re

leva

nt a

spec

ts (

e.g.

the

hom

ogen

eity

re

sults

of

othe

r pe

stic

ides

spi

ked

at t

he s

ame

time,

the

ove

rall

dist

ribut

ion

of t

he p

artic

ipan

ts’

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 6

of 1

6

resu

lts, t

he a

naly

tical

diff

icul

ties

face

d du

ring

the

test

, kno

wle

dge

of th

e an

alyt

ical

beh

avio

ur o

f the

pe

stic

ide

ques

tion)

may

dec

ide

to o

verr

ule

the

test

. Th

e re

ason

s of

thi

s ov

erru

ling

have

to

be

trans

pare

ntly

exp

lain

ed in

the

Fina

l EU

PT-R

epor

t.

Stab

ility

of t

he a

naly

tes

cont

aine

d in

the

Test

Item

The

Test

Item

s w

ill al

so b

e te

sted

for

stab

ility

- ac

cord

ing

to IS

O 1

3528

, Ann

ex B

. The

tim

e de

lay

betw

een

the

first

and

the

last

sta

bilit

y te

st m

ust e

xcee

d th

e pe

riod

of th

e EU

PT-e

xerc

ise.

Typ

ical

ly

the

first

ana

lysi

s is

car

ried

out

shor

tly b

efor

e th

e sh

ipm

ent

of t

he T

est

Item

s an

d th

e la

st o

ne

shor

tly a

fter

the

dead

line

for

subm

issi

on o

f res

ults

. To

bette

r re

cogn

ise

trend

s an

d ga

in a

dditi

onal

ce

rtain

ty o

ne o

r mor

e ad

ditio

nal t

ests

may

be

cond

ucte

d by

the

Org

anis

ers.

At l

east

6 s

ub-s

ampl

es

(ana

lytic

al p

ortio

ns) s

houl

d be

ana

lyse

d on

eac

h te

st d

ay (e

.g. 2

ana

lytic

al p

ortio

ns w

ithdr

awn

from

th

ree

rand

omly

cho

sen

cont

aine

rs O

R 6

por

tions

with

draw

n fro

m a

sin

gle

cont

aine

r). In

prin

cipl

e al

l pe

stic

ides

con

tain

ed in

the

Test

Item

sho

uld

be c

heck

ed fo

r sta

bilit

y. H

owev

er, i

n in

divi

dual

cas

es,

whe

re s

uffic

ient

kno

wle

dge

exis

ts t

hat

the

stab

ility

of a

cer

tain

ana

lyte

is

very

unl

ikel

y to

be

sign

ifica

ntly

af

fect

ed

durin

g st

orag

e (e

.g.

base

d on

ex

perie

nce

from

pa

st

stab

ility

test

s or

kn

owle

dge

of it

s ph

ysic

oche

mic

al p

rope

rties

), th

e O

rgan

iser

s, a

fter

cons

ulta

tion

with

the

EU

PT-

QC

G, m

ay d

ecid

e to

om

it a

spec

ific

stab

ility

test

. The

EU

PT-S

C w

ill fin

ally

dec

ide

whe

ther

ana

lyte

s fo

r w

hich

the

sta

bilit

y te

st w

as n

ot u

nder

take

n w

ill be

incl

uded

in t

he f

inal

rep

ort,

cons

ider

ing

all

rele

vant

asp

ects

suc

h as

the

dist

ribut

ion

of th

e pa

rtici

pant

’s re

sults

(CV*

).

A pe

stic

ide

is c

onsi

dere

d to

be

adeq

uate

ly s

tabl

e if

| yi -y

| ≤ 0.

3×σ p

t, w

here

yi th

e m

ean

valu

e of

the

last

per

iod

of th

e st

abilit

y te

st, y

is th

e m

ean

valu

e of

the

first

per

iod

of th

e st

abilit

y te

st a

nd σ

pt th

e st

anda

rd d

evia

tion

used

for p

rofic

ienc

y as

sess

men

t (ty

pica

lly 2

5% o

f the

ass

igne

d va

lue)

.

The

resu

lts o

f all

stab

ility

test

s ar

e pr

esen

ted

to th

e EU

PT-S

C. I

n sp

ecia

l cas

es w

here

the

abov

e st

abilit

y te

st c

riter

ia a

re n

ot m

et,

the

EUPT

-SC

con

side

ring

all

rele

vant

asp

ects

(e.

g. t

he p

ast

expe

rienc

e w

ith th

e st

abilit

y of

the

com

poun

d, th

e ov

eral

l dis

tribu

tion

the

parti

cipa

nts’

res

ults

, the

m

easu

rem

ent

varia

bilit

y, a

naly

tical

diff

icul

ties

face

d du

ring

the

test

and

kno

wle

dge

abou

t th

e an

alyt

ical

beh

avio

ur o

f the

pes

ticid

e qu

estio

n) m

ay d

ecid

e to

ove

rrul

e th

e te

st. T

he re

ason

s of

this

ov

erru

ling

will

be tr

ansp

aren

tly e

xpla

ined

in th

e Fi

nal E

UPT

-Rep

ort.

The

Org

anis

ers

may

als

o de

cide

to c

ondu

ct a

dditi

onal

sta

bilit

y te

sts

at d

iffer

ent s

tora

ge c

ondi

tions

th

an th

ose

reco

mm

ende

d to

the

parti

cipa

nts

e.g.

at a

mbi

ent t

empe

ratu

re.

Con

side

ring

know

ledg

e ab

out t

he e

xpec

ted

susc

eptib

ility

of p

estic

ides

in th

e Te

st It

em to

pos

sibl

e lo

sses

, th

e O

rgan

iser

s w

ill ch

oose

the

shi

pmen

t co

nditi

ons

to b

e su

ch t

hat

pest

icid

e lo

sses

are

m

inim

ised

(e.

g. s

hipm

ent

of f

roze

n sa

mpl

es,

addi

tion

of d

ry i

ce).

As s

hipm

ent

time

can

diffe

r


A-42


8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 7

of 1

6

betw

een

labs

/cou

ntrie

s it

is r

ecom

men

ded

that

the

Org

anis

ers

cond

uct a

dditi

onal

sta

bilit

y te

sts

at

cond

ition

s si

mul

atin

g sh

ipm

ent.

Shou

ld c

ritic

al lo

sses

be

dete

cted

for c

erta

in p

estic

ides

the

EUPT

-SC

will

be in

form

ed (o

r the

EU

PT-Q

CG

bef

ore

or d

urin

g th

e te

st).

Cas

e-by

-cas

e de

cisi

ons

may

be

take

n co

nsid

erin

g al

l re

leva

nt a

spec

ts i

nclu

ding

the

shi

pmen

t tim

e of

the

sam

ples

to

each

la

bora

tory

.

Met

hodo

logi

es to

be

used

by

the

part

icip

ants

Parti

cipa

ting

labo

rato

ries

are

inst

ruct

ed to

use

the

anal

ytic

al p

roce

dure

(s) t

hat t

hey

wou

ld r

outin

ely

empl

oy in

offi

cial

con

trol a

ctiv

ities

(m

onito

ring

etc.

). W

here

an

anal

ytic

al m

etho

d ha

s no

t yet

bee

n es

tabl

ishe

d ro

utin

ely

this

sho

uld

be s

tate

d.

Gen

eral

pro

cedu

res

for r

epor

ting

resu

lts

Parti

cipa

ting

labo

rato

ries

are

resp

onsi

ble

for

repo

rting

th

eir

own

quan

titat

ive

resu

lts

to

the

Org

anis

er w

ithin

the

stip

ulat

ed d

eadl

ine.

Any

pes

ticid

e th

at w

as t

arge

ted

by a

par

ticip

atin

g la

bora

tory

sho

uld

be re

porte

d as

“ana

lyse

d”. E

ach

labo

rato

ry w

ill be

abl

e to

rep

ort o

nly

one

resu

lt fo

r eac

h an

alyt

e de

tect

ed in

the

Test

Item

. The

con

cent

ratio

ns o

f the

pes

ticid

es d

etec

ted

shou

ld b

e ex

pres

sed

in ‘m

g/kg

’ unl

ess

indi

cate

d ot

herw

ise

in th

e sp

ecifi

c pr

otoc

ol.

The

Test

Ite

m is

inte

ntio

nally

tre

ated

with

pes

ticid

es w

here

as t

he B

lank

Mat

eria

l is

anal

ysed

to

ensu

re th

at it

doe

s no

t con

tain

any

of t

he p

estic

ides

in th

e Ta

rget

Pes

ticid

es L

ist,

at o

r abo

ve, t

he

spec

ified

MR

RLs

. Bot

h th

e Te

st It

em a

nd B

lank

Mat

eria

l hav

e to

be

anal

ysed

by

the

parti

cipa

ting

labo

rato

ries

and

any

pest

icid

e de

tect

ed in

them

mus

t be

repo

rted.

Cor

rect

ion

of re

sults

for r

ecov

ery

Acco

rdin

g to

the

Met

hod

Valid

atio

n an

d Q

ualit

y C

ontro

l Pr

oced

ures

for

Pes

ticid

e R

esid

ues

Anal

ysis

in F

ood

and

Feed

8 , it

is c

omm

on p

ract

ice

that

pes

ticid

e an

alys

is re

sults

are

not

cor

rect

ed

for r

ecov

ery

if th

e re

cove

ry ra

tes

rang

e be

twee

n 70

and

120

%. C

orre

ctio

n of

resu

lts fo

r rec

over

y is

re

com

men

ded

if th

e av

erag

e re

cove

ry is

sig

nific

antly

diff

eren

t fro

m 1

00 %

(ty

pica

lly if

out

side

the

70 –

120

%

rang

e).

Appr

oach

es

for

reco

very

co

rrec

tion

expl

icitl

y st

ated

in

th

e D

G-S

ANTE

do

cum

ent a

re th

e us

e of

rec

over

y co

rrec

tion

fact

ors,

the

use

of s

tabl

e is

otop

e la

belle

d an

alog

ues

8 Doc

umen

t N°

SA

NTE

/118

13/2

017;

Met

hod

Valid

atio

n an

d Q

ualit

y C

ontro

l Pro

cedu

res

for P

estic

ide

Res

idue

s An

alys

is

in F

ood

and

Feed

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 8

of 1

6

of th

e ta

rget

ana

lyte

s as

Inte

rnal

Sta

ndar

ds (I

LIS

s), t

he ‘p

roce

dura

l cal

ibra

tion’

app

roac

h as

wel

l as

the

appr

oach

of ‘

stan

dard

add

ition

’ with

add

ition

s of

ana

lyte

(s)

bein

g m

ade

to a

naly

tical

por

tions

. R

esul

ts m

ay b

e co

rrect

ed f

or r

ecov

ery

only

in c

ases

whe

re t

his

corre

ctio

n is

app

lied

in r

outin

e pr

actic

e (in

clud

ing

case

s of

MR

L-vi

olat

ions

). La

bora

torie

s ar

e re

quire

d to

rep

ort

whe

ther

the

ir re

sults

wer

e ad

just

ed f

or r

ecov

ery

and,

if

a re

cove

ry f

acto

r w

as u

sed,

the

rec

over

y ra

te (

in

perc

enta

ge) m

ust a

lso

be re

porte

d. N

o re

cove

ry d

ata

are

requ

ired

whe

re c

orre

ctio

n fo

r rec

over

y is

au

tom

atic

by

addi

ng a

mou

nts

of a

naly

tes

to t

he t

est

porti

on f

or u

sing

the

‘st

anda

rd a

dditi

on’

appr

oach

, or

isot

opic

ally

-labe

lled

inte

rnal

sta

ndar

ds (

in b

oth

case

s w

ith s

piki

ng in

to th

e Te

st It

em

at t

he b

egin

ning

of

the

extra

ctio

n pr

oced

ures

) or

pro

cedu

ral

calib

ratio

n. I

n th

ese

case

s, t

he

labo

rato

ries

shou

ld re

port

the

actu

al a

ppro

ach

that

was

follo

wed

.

Met

hodo

logy

info

rmat

ion

All l

abor

ator

ies

are

requ

este

d to

pro

vide

info

rmat

ion

on th

e an

alyt

ical

met

hod(

s) th

ey h

ave

used

. A

com

pila

tion

of th

e m

etho

dolo

gy in

form

atio

n su

bmitt

ed b

y al

l par

ticip

ants

is p

rese

nted

in a

n An

nex

of t

he f

inal

rep

ort

or i

n a

sepa

rate

rep

ort.

Whe

re n

eces

sary

the

met

hods

are

eva

luat

ed a

nd

disc

usse

d, e

spec

ially

in t

hose

cas

es w

here

the

res

ult

dist

ribut

ion

is n

ot u

nim

odal

or

very

bro

ad

(e.g

. CV*

> 3

5 %

). If

no s

uffic

ient

info

rmat

ion

on th

e m

etho

dolo

gy u

sed

is p

rovi

ded,

the

Org

anis

er

rese

rves

the

rig

ht n

ot t

o ac

cept

the

ana

lytic

al r

esul

ts r

epor

ted

by t

he p

artic

ipan

ts c

once

rned

or

even

refu

se p

artic

ipat

ion

in th

e fo

llow

ing

PT.

Res

ults

eva

luat

ion

The

proc

edur

es u

sed

for t

he tr

eatm

ent a

nd a

sses

smen

t of r

esul

ts a

re d

escr

ibed

bel

ow.

Fals

e Po

sitiv

e re

sults

Thes

e ar

e re

sults

of p

estic

ides

from

the

Targ

et P

estic

ides

Lis

t, th

at a

re re

porte

d, a

t or a

bove

, the

ir re

spec

tive

MR

RL

alth

ough

the

y w

ere:

(i)

not

dete

cted

by

the

Org

anis

er,

even

afte

r re

peat

ed

anal

yses

, an

d/or

(ii)

not

det

ecte

d by

the

ove

rwhe

lmin

g m

ajor

ity (

e.g.

> 9

5 %

) of

the

par

ticip

atin

g la

bora

torie

s th

at h

ad ta

rget

ed th

e sp

ecifi

c pe

stic

ides

. In

certa

in in

stan

ces,

cas

e-by

-cas

e de

cisi

ons

by th

e EU

PT-P

anel

may

be

nece

ssar

y.

Any

resu

lts r

epor

ted

low

er th

an th

e M

RR

L w

ill no

t be

cons

ider

ed a

s fa

lse

posi

tives

, eve

n th

ough

th

ese

resu

lts s

houl

d no

t hav

e be

en re

porte

d.


A-43


A8

Gen

erA

l Pro

toco

(8th

ed

.)

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 9

of 1

6

Fals

e N

egat

ive

resu

lts

Thes

e ar

e re

sults

for

pes

ticid

es r

epor

ted

by t

he la

bora

torie

s as

’ana

lyse

d’ b

ut w

ithou

t re

porti

ng

num

eric

al v

alue

s al

thou

gh t

hey

wer

e: a

) us

ed b

y th

e O

rgan

iser

to

treat

the

Tes

t Ite

m a

nd b

) de

tect

ed b

y th

e O

rgan

iser

as

wel

l as

the

maj

ority

of

the

parti

cipa

nts

that

had

tar

gete

d th

ese

spec

ific

pest

icid

es a

t or

abov

e th

e re

spec

tive

MR

RLs

. R

esul

ts r

epor

ted

as ’<

RL’

(R

L= R

epor

ting

Lim

it of

the

labo

rato

ry) w

ill be

con

side

red

as n

ot d

etec

ted

and

will

be ju

dged

as

fals

e ne

gativ

es. I

n ce

rtain

inst

ance

s, c

ase-

by-c

ase

deci

sion

s by

the

EUPT

-Pan

el m

ay b

e ne

cess

ary.

In c

ases

of t

he a

ssig

ned

valu

e be

ing

less

than

a fa

ctor

of 3

tim

es th

e M

RR

L, fa

lse

nega

tives

will

ty

pica

lly n

ot b

e as

sign

ed.

The

EUPT

-Pan

el m

ay d

ecid

e to

tak

e ca

se-b

y-ca

se d

ecis

ions

in

this

re

spec

t afte

r co

nsid

erin

g al

l rel

evan

t fac

tors

suc

h as

the

resu

lt di

strib

utio

n an

d th

e re

porti

ng li

mits

of

the

affe

cted

labs

.

Es

timat

ion

of th

e as

sign

ed v

alue

(xpt

)

In o

rder

to

min

imis

e th

e in

fluen

ce o

f ou

t-lyi

ng r

esul

ts o

n th

e st

atis

tical

eva

luat

ion,

the

ass

igne

d va

lue

x pt

(= c

onse

nsus

con

cent

ratio

n) w

ill ty

pica

lly b

e es

timat

ed u

sing

rob

ust

estim

ate

of t

he

parti

cipa

nt’s

mea

n (x

*) a

s de

scrib

ed in

ISO

135

28:2

0159 ,

taki

ng in

to a

ccou

nt th

e re

sults

rep

orte

d by

EU

and

EFT

A co

untri

es l

abor

ator

ies

only

. In

spe

cial

jus

tifia

ble

case

s, t

he E

UPT

-Pan

el m

ay

deci

de t

o el

imin

ate

certa

in r

esul

ts t

race

ably

ass

ocia

ted

with

gro

ss e

rrors

(se

e “O

mis

sion

or

Excl

usio

n of

resu

lts” b

elow

) or t

o us

e on

ly th

e re

sults

of a

sub

grou

p co

nsis

ting

of la

bora

torie

s th

at

have

repe

ated

ly d

emon

stra

ted

good

per

form

ance

for t

he s

peci

fic c

ompo

und

in th

e pa

st.

O

mis

sion

or E

xclu

sion

of r

esul

ts

Befo

re e

stim

atin

g th

e as

sign

ed v

alue

res

ults

ass

ocia

ted

with

obv

ious

mis

take

s ha

ve t

o be

ex

amin

ed to

dec

ide

whe

ther

they

sho

uld

be r

emov

ed fr

om th

e po

pula

tion.

Suc

h gr

oss

erro

rs m

ay

incl

ude

inco

rrec

t rec

ordi

ng (

e.g.

due

to tr

ansc

riptio

n er

rors

by

the

parti

cipa

nt, d

ecim

al p

oint

faul

ts

or t

rans

pose

d di

gits

, in

corr

ect

unit)

, ca

lcul

atio

n er

rors

(e.

g. m

issi

ng f

acto

rs),

anal

ysis

of

a w

rong

sa

mpl

e/ex

tract

(e.

g. a

spi

ked

blan

k), u

se o

f wro

ng c

once

ntra

tions

of s

tand

ard

solu

tions

, inc

orre

ct

9 D

IN I

SO

135

28:2

015,

Sta

tistic

al m

etho

ds f

or u

se in

pro

ficie

ncy

test

ing

by in

terla

bora

tory

com

paris

ons,

Int

erna

tiona

l O

rgan

izat

ion

for

Sta

ndar

diza

tion.

The

rein

a s

peci

fic r

obus

t m

etho

d fo

r de

term

inat

ion

of t

he c

onse

nsus

mea

n an

d st

anda

rd d

evia

tion

with

out t

he n

eed

for r

emov

al o

f dev

iatin

g re

sults

is d

escr

ibed

(Alg

orith

m A

in A

nnex

C).

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 10

of 1

6

data

pro

cess

ing

(e.g

. int

egra

tion

of w

rong

pea

k), m

ajor

dev

iatio

ns fr

om th

e an

alyt

ical

pro

cedu

re,

inap

prop

riate

sto

rage

or

trans

port

cond

ition

s (in

cas

e of

sus

cept

ible

com

poun

ds),

and

the

use

of

inap

prop

riate

pro

cedu

res

that

dem

onst

rabl

y le

ad t

o si

gnifi

cant

ly b

iase

d re

sults

(e.

g. d

ue t

o de

grad

atio

n or

inc

ompl

ete

extra

ctio

n).

Whe

re t

he O

rgan

iser

s (e

.g.

afte

r th

e pu

blic

atio

n of

the

pr

elim

inar

y re

port)

rec

eive

inf

orm

atio

n of

suc

h gr

oss

erro

rs,

havi

ng a

sig

nific

ant

impa

ct o

n a

gene

rate

d re

sult,

the

affe

cted

resu

lts w

ill be

exa

min

ed o

n a

case

-by-

case

bas

is to

dec

ide

whe

ther

, or

not

, the

y sh

ould

be

excl

uded

from

the

popu

latio

n us

ed fo

r rob

ust s

tatis

tics.

Res

ults

may

als

o be

om

itted

e.g

. if a

n in

appr

opria

te m

etho

d ha

s be

en u

sed

even

if th

ey a

re n

ot o

utlie

rs.

All d

ecis

ions

to

omit/

excl

ude

resu

lts w

ill be

dis

cuss

ed w

ith t

he E

UPT

-SC

and

the

rea

soni

ng f

or t

he o

mis

sion

of

each

res

ult

clea

rly s

tate

d in

the

fin

al E

UPT

-Rep

ort.

How

ever

, z

scor

es w

ill be

cal

cula

ted

for

all

resu

lts ir

resp

ectiv

e of

the

fact

that

they

wer

e om

itted

from

the

calc

ulat

ion

of th

e as

sign

ed v

alue

.

Om

itted

res

ults

mig

ht b

e in

tere

stin

g as

the

y m

ight

giv

e in

dica

tions

abo

ut p

ossi

ble

sour

ce(s

) of

er

rors

. The

Org

anis

ers

will

thus

ask

the

rele

vant

lab(

s) to

pro

vide

feed

back

on

poss

ible

sou

rces

of

erro

rs (s

ee a

lso

“follo

w-u

p ac

tiviti

es”).

Unc

erta

inty

of t

he a

ssig

ned

valu

e

The

unce

rtain

ty o

f the

ass

igne

d va

lues

u(x

pt) i

s ca

lcul

ated

acc

ordi

ng to

ISO

135

28:2

015

as:

𝑢𝑢 (𝑥𝑥

𝑝𝑝𝑝𝑝)=

1,25×

𝑠𝑠∗ √𝑝𝑝

whe

re s*

is th

e ro

bust

sta

ndar

d de

viat

ion

and 𝑝𝑝

is th

e nu

mbe

r of r

esul

ts.

In c

erta

in c

ases

, and

con

side

ring

all r

elev

ant f

acto

rs (e

.g. t

he re

sult

dist

ribut

ion,

mul

timod

ality

), th

e nu

mbe

r of

sub

mitt

ed r

esul

ts,

info

rmat

ion

rega

rdin

g an

alyt

e ho

mog

enei

ty/s

tabi

lity,

inf

orm

atio

n re

gard

ing

the

use

of m

etho

dolo

gies

that

mig

ht p

rodu

ce a

bia

s th

at w

ere

used

by

the

parti

cipa

nts)

, th

e EU

PT-P

anel

may

con

side

r th

e as

sign

ed v

alue

of

a sp

ecifi

c an

alyt

e to

be

too

unce

rtain

and

de

cide

tha

t th

e re

sults

sho

uld

not

be e

valu

ated

, or

onl

y ev

alua

ted

for

info

rmat

ive

purp

oses

. The

pr

ovis

ions

of I

SO 1

3528

:201

5 co

ncer

ning

the

unce

rtain

ty o

f the

ass

igne

d va

lue

will

be ta

ken

into

ac

coun

t.

St

anda

rd d

evia

tion

of th

e as

sign

ed v

alue

(tar

get s

tand

ard

devi

atio

n)

The

targ

et s

tand

ard

devi

atio

n of

the

ass

igne

d va

lue

(FFP

- σpt)

will

be c

alcu

late

d us

ing

a Fi

t-For

-Pu

rpos

e ap

proa

ch w

ith a

fixe

d R

elat

ive

Stan

dard

Dev

iatio

n (F

FP-R

SD) o

f 25%

as

follo

ws:


A-44


8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 11

of 1

6

FFP-σ p

t = 0.

25 ×

x pt

Th

e pe

rcen

tage

FFP

-RSD

is s

et a

t 25%

bas

ed o

n ex

perie

nce

from

res

ults

of

prev

ious

EU

PTs10

. Th

e EU

PT-P

anel

res

erve

s th

e rig

ht t

o al

so e

mpl

oy o

ther

app

roac

hes

on a

cas

e-by

-cas

e ba

sis

cons

ider

ing

anal

ytic

al d

iffic

ultie

s an

d ex

perie

nce

gain

ed fr

om p

revi

ous

prof

icie

ncy

test

s.

For i

nfor

mat

ive

purp

oses

the

robu

st re

lativ

e st

anda

rd d

evia

tion

(CV*

) is

calc

ulat

ed a

ccor

ding

to IS

O

1352

8:20

15;

Cha

pter

7.7

(C

onse

nsus

val

ue f

rom

par

ticip

ant

resu

lts)

follo

win

g Al

gorit

hm A

in

Anne

x C

.

z

scor

es

This

par

amet

er is

cal

cula

ted

usin

g th

e fo

llow

ing

form

ula:

𝑧𝑧 𝑖𝑖=(𝑥𝑥

𝑖𝑖−𝑥𝑥 𝑝𝑝

𝑝𝑝)𝐹𝐹𝐹𝐹

𝐹𝐹-𝜎𝜎 𝑝𝑝

𝑝𝑝

whe

re x

i is

the

valu

e re

porte

d by

the

lab

orat

ory,

xpt

is

the

assi

gned

val

ue,

and

FFP-σ p

t is

the

st

anda

rd d

evia

tion

usin

g FF

P ap

proa

ch.

Z sc

ores

will

be r

ound

ed t

o on

e de

cim

al p

lace

. Fo

r th

e ca

lcul

atio

n of

com

bine

d z

scor

es (s

ee b

elow

) the

orig

inal

z s

core

s w

ill be

use

d an

d ro

unde

d to

one

de

cim

al p

lace

afte

r cal

cula

tion.

Any

z sc

ores

> 5

will

be t

ypic

ally

rep

orte

d as

‘> 5

’ and

a v

alue

of

‘5’ w

ill be

use

d to

cal

cula

te

com

bine

d z

scor

es (s

ee b

elow

).

Z sc

ores

will

be in

terp

rete

d in

the

follo

win

g w

ay, a

s is

set

in th

e IS

O 1

7043

:201

011:

|z

| 2

.0

Ac

cept

able

2.

0

|z| <

3.0

Que

stio

nabl

e

|z

| ≥ 3

.0

U

nacc

epta

ble

For r

esul

ts c

onsi

dere

d as

fals

e ne

gativ

es, z

sco

res

will

be c

alcu

late

d us

ing

the

MR

RL

or R

L (th

e la

bora

tory

’s R

epor

ting

Lim

it) if

the

RL

< M

RR

L. T

he E

UPT

-Pan

el w

ill de

cide

whe

ther

, or n

ot, t

hese

va

lues

sho

uld

appe

ar in

the

z sc

ore

hist

ogra

ms.

10 C

ompa

rativ

e S

tudy

of t

he M

ain

Top-

dow

n A

ppro

ache

s fo

r th

e E

stim

atio

n of

Mea

sure

men

t Unc

erta

inty

in M

ultir

esid

ue

Ana

lysi

s of

Pes

ticid

es in

Fru

its a

nd V

eget

able

s. J

. Agr

ic. F

ood

Che

m.,

2011

, 59(

14),

7609

-761

9.

11 IS

O/IE

C 1

7043

:201

0. C

onfo

rmity

ass

essm

ent –

Gen

eral

requ

irem

ents

for p

rofic

ienc

y te

stin

g

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 12

of 1

6

C

ateg

ory

A a

nd B

cla

ssifi

catio

n

The

EUPT

-Pan

el w

ill de

cide

if a

nd h

ow t

o cl

assi

fy t

he la

bora

torie

s in

to tw

o ca

tego

ries

- A

or B

. C

urre

ntly

, la

bora

torie

s th

at a

re a

ble

to a

naly

se a

t le

ast

90%

of

the

com

puls

ory

pest

icid

es in

the

ta

rget

pes

ticid

es li

st,

have

cor

rect

ly d

etec

ted

and

quan

tifie

d a

suffi

cien

tly h

igh

perc

enta

ge o

f th

e pe

stic

ides

pre

sent

in

the

Test

Ite

m (

at l

east

90

%)

and

repo

rted

no f

alse

pos

itive

s w

ill ha

ve

dem

onst

rate

d ‘s

uffic

ient

sco

pe’

and

can

ther

efor

e be

cla

ssifi

ed i

nto

Cat

egor

y A.

For

the

90%

cr

iterio

n th

e nu

mbe

r of p

estic

ides

nee

ded

to b

e co

rrec

tly a

naly

sed

to h

ave

suffi

cien

t sco

pe w

ill be

ca

lcul

ated

by

mul

tiply

ing

the

num

ber

of c

ompu

lsor

y pe

stic

ides

from

the

Targ

et P

estic

ides

Lis

t by

0.9

and

roun

ding

to

the

near

est

full

num

ber

with

0.5

dec

imal

s be

ing

roun

ded

dow

nwar

ds (

see

som

e ex

ampl

es in

Tab

le 1

).

Tabl

e 1.

No.

of p

estic

ides

from

the

Targ

et P

estic

ides

Lis

t nee

ded

to b

e ta

rget

ed o

r pes

ticid

es p

rese

nt

in th

e Te

st It

em th

at n

eed

to b

e co

rrec

tly d

etec

ted

and

quan

tifie

d to

hav

e su

ffici

ent s

cope

.

No.

of c

ompu

lsor

y pe

stic

ides

pre

sent

in th

e Te

st It

em /

Targ

et

Pest

icid

es L

ist (

N)

90 %

N

o. o

f pes

ticid

es n

eede

d to

be

corr

ectly

det

ecte

d an

d qu

antif

ied

/ tar

gete

d to

hav

e su

ffici

ent

scop

e (n

) n

3 2.

7 3

N

4 3.

6 4

5 4.

5 4

N -

1

6 5.

4 5

7 6.

3 6

8 7.

2 7

9 8.

1 8

10

9.0

9 11

9.

9 10

12

10

.8

11

13

11.7

12

14

12

.6

13

15

13.5

13

N -

2

16

14.4

14

17

15

.3

15

18

16.2

16

19

17

.1

17

20

18

18

21

18.9

19

22

19

.8

20

23

20.7

21

24

21

.6

22

25

22.5

22

N

- 3

26

23.4

23


A-45


A8

Gen

erA

l Pro

toco

(8th

ed

.)

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 13

of 1

6

O

vera

ll pe

rfor

man

ce o

f lab

orat

orie

s - c

ombi

ned

z sc

ores

For

eval

uatio

n of

the

ove

rall

perfo

rman

ce o

f la

bora

torie

s w

ithin

Cat

egor

y A

, th

e Av

erag

e of

the

Sq

uare

d z

scor

e (A

Z2 )12

,13 (

see

belo

w) w

ill be

use

d. T

he A

Z2 is

calc

ulat

ed a

s fo

llow

s:

nzAZ

n ii

1

2

2

Whe

re n

is th

e nu

mbe

r of z

sco

res

to b

e co

nsid

ered

in th

e ca

lcul

atio

n. In

the

calc

ulat

ion

of th

e AZ

2 , z

scor

es h

ighe

r th

an 5

will

be s

et a

s 5.

Bas

ed o

n th

e AZ

2 ac

hiev

ed, t

he la

bora

torie

s are

cla

ssifi

ed

as fo

llow

s:

AZ

2 2

.0

G

ood

2.

0

AZ2 <

3.0

Satis

fact

ory

AZ

2 ≥ 3

.0

U

nsat

isfa

ctor

y

Com

bine

d z

scor

es a

re c

onsi

dere

d to

be

of le

sser

impo

rtanc

e th

an t

he in

divi

dual

z s

core

s. T

he

EUPT

-Pan

el r

etai

ns t

he r

ight

not

to

calc

ulat

e AZ

2 if

it is

con

side

red

as n

ot b

eing

use

ful o

r if

the

num

ber o

f res

ults

repo

rted

by a

ny p

artic

ipan

t is

cons

ider

ed to

be

too

low

.

In th

e ca

se o

f EU

PT-S

RM

s, w

here

onl

y a

few

resu

lts p

er la

b m

ay b

e av

aila

ble,

the

Aver

age

of th

e Ab

solu

te z

sco

res

(AAZ

) m

ay b

e ca

lcul

ated

for

info

rmat

ive

purp

oses

, bu

t on

ly f

or la

bs t

hat h

ave

repo

rted

enou

gh r

esul

ts t

o ob

tain

5 o

r m

ore

z sc

ores

. Fo

r th

e ca

lcul

atio

n of

the

AAZ

, z

scor

es

high

er th

an 5

will

also

be

set a

s 5.

Labo

rato

ries

with

in C

ateg

ory

B w

ill be

rank

ed a

ccor

ding

to th

e to

tal n

umbe

r of p

estic

ides

that

they

co

rrec

tly re

porte

d to

be

pres

ent i

n th

e Te

st It

em. T

he n

umbe

r of a

ccep

tabl

e z

scor

es a

chie

ved

will

be p

rese

nted

, too

. The

EU

RL-

Pane

l ret

ains

the

right

to c

alcu

late

com

bine

d z

scor

es (

see

abov

e)

also

for

labs

with

in C

ateg

ory

B, e

.g. f

or in

form

ativ

e pu

rpos

es, p

rovi

ded

that

a m

inim

um n

umbe

r of

resu

lts (z

sco

res)

hav

e be

en re

porte

d.

12 F

orm

erly

nam

ed “S

um o

f squ

ared

z s

core

s (S

Z2 )”

13 L

abor

ator

y as

sess

men

t by

com

bine

d z

scor

e va

lues

in p

rofic

ienc

y te

sts:

exp

erie

nce

gain

ed t

hrou

gh t

he E

UP

T fo

r pe

stic

ide

resi

dues

in fr

uits

and

veg

etab

les.

Ana

l. B

ioan

al. C

hem

., 20

10, 3

97, 3

061–

3070

.

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 14

of 1

6

Publ

icat

ion

of re

sults

The

EUR

Ls w

ill pu

blis

h a

prel

imin

ary

repo

rt, c

onta

inin

g te

ntat

ive

assi

gned

val

ues

and

z sc

ore

valu

es f

or a

ll pe

stic

ides

pre

sent

in

the

Test

Ite

m,

with

in 2

mon

ths

of t

he d

eadl

ine

for

resu

lt su

bmis

sion

.

The

Fina

l EU

PT R

epor

t will

be p

ublis

hed

afte

r th

e EU

PT-P

anel

has

dis

cuss

ed th

e re

sults

. Tak

ing

into

acc

ount

tha

t th

e EU

PT-P

anel

mee

ts n

orm

ally

onl

y on

ce a

yea

r (ty

pica

lly in

late

sum

mer

or

autu

mn)

to d

iscu

ss th

e re

sults

of a

ll EU

PTs

orga

nise

d by

the

EUR

Ls e

arlie

r in

the

year

, the

fina

l re

port

may

be

publ

ishe

d up

to

10 m

onth

s af

ter

the

dead

line

for

resu

lts s

ubm

issi

on.

Res

ults

su

bmitt

ed b

y no

n-EU

/EFT

A la

bora

torie

s m

ight

not

alw

ays

be u

sed

in t

he t

able

s or

fig

ures

in t

he

final

repo

rt.

Cer

tific

ates

of p

artic

ipat

ion

Toge

ther

with

the

Fina

l EU

PT-R

epor

t, th

e EU

RL

Org

anis

er w

ill de

liver

a C

ertif

icat

e of

Par

ticip

atio

n to

eac

h pa

rtici

patin

g la

bora

tory

sho

win

g th

e z

scor

es a

chie

ved

for

each

indi

vidu

al p

estic

ide,

the

co

mbi

ned

z sc

ores

cal

cula

ted

(if a

ny),

and

the

clas

sific

atio

n in

to C

ateg

ory

A or

B.

Feed

back

At a

ny ti

me

befo

re, d

urin

g or

afte

r the

PT

parti

cipa

nts

have

the

poss

ibilit

y to

con

tact

the

Org

anis

ers

and

mak

e su

gges

tions

or

in

dica

te

erro

rs.

Afte

r th

e di

strib

utio

n of

th

e Fi

nal

EUPT

-Rep

ort,

parti

cipa

ting

labo

rato

ries

will

be g

iven

the

oppo

rtuni

ty to

giv

e th

eir f

eedb

ack

to th

e O

rgan

iser

s an

d m

ake

sugg

estio

ns fo

r fut

ure

impr

ovem

ents

.

Cor

rect

ion

of e

rror

s

Shou

ld e

rror

s be

dis

cove

red

in a

ny o

f the

doc

umen

ts is

sued

prio

r to

the

EUPT

(C

alen

dar,

Targ

et

Pest

icid

es L

ist,

Spec

ific

Prot

ocol

, Gen

eral

Pro

toco

l) th

e co

rrect

ed d

ocum

ents

will

be u

ploa

ded

onto

th

e w

ebsi

te a

nd in

the

case

of s

ubst

antia

l erro

rs th

e pa

rtici

pant

s w

ill be

info

rmed

. Bef

ore

star

ting

the

exer

cise

par

ticip

ants

sho

uld

mak

e su

re t

o do

wnl

oad

the

late

st v

ersi

on o

f th

ese

docu

men

ts.

If su

bsta

ntia

l erro

rs a

re d

isco

vere

d in

the

Prel

imin

ary

EUPT

-Rep

ort t

he O

rgan

iser

s w

ill di

strib

ute

a ne

w c

orre

cted

ver

sion

, whe

re it

will

be s

tate

d th

at th

e pr

evio

us v

ersi

on is

no

long

er v

alid

.


A-46


8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 15

of 1

6

Whe

re s

ubst

antia

l er

rors

are

dis

cove

red

in t

he F

inal

EU

PT-R

epor

t th

e EU

PT-P

anel

will

deci

de

whe

ther

a c

orrig

endu

m w

ill be

issu

ed a

nd h

ow t

his

shou

ld lo

ok.

The

onlin

e ve

rsio

n of

the

fin

al

repo

rt w

ill be

repl

aced

by

the

new

one

and

all

affe

cted

labs

will

be c

onta

cted

.

Whe

re e

rror

s ar

e di

scov

ered

in

EUPT

-Cer

tific

ates

the

rel

evan

t la

bora

torie

s w

ill be

sen

t ne

w

corr

ecte

d on

es. W

here

nec

essa

ry th

e la

bora

torie

s w

ill be

ask

ed to

retu

rn th

e ol

d on

es.

Follo

w-u

p ac

tiviti

es

Labo

rato

ries

are

expe

cted

to u

nder

take

follo

w-u

p ac

tiviti

es to

trac

e ba

ck th

e so

urce

s of

erro

neou

s or

stro

ngly

dev

iatin

g re

sults

(ty

pica

lly t

hose

with

|z|

> 2

.0)

- in

clud

ing

all

fals

e po

sitiv

es.

Even

re

sults

with

in |z

| ≤

2.0

may

hav

e to

be

chec

ked

if th

ere

is in

dica

tions

of

a si

gnifi

cant

pos

itive

or

nega

tive

bias

.

Upo

n re

ques

t, th

e la

bora

tory

’s c

orre

spon

ding

NR

L an

d EU

RL

are

to b

e in

form

ed o

f the

out

com

e of

an

y in

vest

igat

ive

activ

ities

for

fal

se p

ositi

ves,

fal

se n

egat

ives

and

for

res

ults

with

|z|

≥ 3

.0.

Con

cern

ing

z sc

ores

bet

wee

n 2.

0 an

d 3.

0 th

e co

mm

unic

atio

n of

the

outc

ome

of fo

llow

-up

activ

ities

is

opt

iona

l but

hig

hly

enco

urag

ed w

here

the

sour

ce o

f dev

iatio

n co

uld

be id

entif

ied

and

coul

d be

of

inte

rest

to o

ther

labs

.

Acco

rdin

g to

inst

ruct

ions

from

DG

-SAN

TE, t

he “P

roto

col f

or m

anag

emen

t of u

nder

perfo

rman

ce in

com

para

tive

test

ing

and/

or la

ck o

f col

labo

ratio

n of

Nat

iona

l Ref

eren

ce L

abor

ator

ies

(NR

Ls) w

ith

EU R

efer

ence

Lab

orat

orie

s (E

UR

Ls) a

ctiv

ities

” is

to b

e fo

llow

ed.

NR

Ls w

ill be

con

side

red

as u

nder

perf

orm

ing

in re

latio

n to

sco

pe if

in a

t lea

st tw

o of

the

last

four

EUPT

s fa

lling

with

in th

eir r

espo

nsib

ility

area

if th

ey: a

) hav

en’t

parti

cipa

ted,

or b

) tar

gete

d le

ss th

an

90%

of t

he c

ompu

lsor

y pe

stic

ides

in th

e ta

rget

list

s (8

0% fo

r SR

M-c

ompo

unds

), or

c) d

etec

ted

less

than

90%

of

the

com

puls

ory

com

poun

ds p

rese

nt i

n th

e te

st i

tem

s (8

0% f

or S

RM

-com

poun

ds).

Addi

tiona

lly,

NR

Ls t

hat

obta

ined

AZ2

high

er t

han

3 in

tw

o co

nsec

utiv

e EU

PTs

of t

he l

ast

four

EUPT

s, w

ill be

con

side

red

as u

nder

perf

orm

ing

in a

ccur

acy.

A tw

o-st

ep p

roto

col e

stab

lishe

d by

DG

-SAN

TE w

ill be

app

lied

as s

oon

as u

nder

perfo

rman

ce o

f an

NR

L is

det

ecte

d14:

Phas

e 1:

Id

entif

ying

the

orig

in o

f the

bad

resu

lts (f

ailu

re in

EU

PTs)

.

14 A

rticl

e 10

1 of

Reg

ulat

ion

(EC

) 625

/201

7

8th

Edi

tion:

Rev

ised

23th

Jan

uary

, 201

8

Pag

e 16

of 1

6

Ac

tions

: On

the

spot

vis

its a

nd tr

aini

ng if

nec

essa

ry a

nd re

petit

ion

of th

e co

mpa

rativ

e te

st if

feas

ible

and

clo

se th

e as

sess

men

t of r

esul

ts b

y th

e E

UR

L.

Phas

e 2:

If

the

resu

lts s

till r

evea

l und

erpe

rform

ance

the

Com

mis

sion

sha

ll be

info

rmed

offi

cial

ly b

y

the

EUR

L in

clud

ing

a re

port

of th

e m

ain

findi

ngs

and

corre

ctiv

e ac

tions

.

Th

e C

omm

issi

on s

hall

info

rm th

e C

ompe

tent

Aut

horit

y an

d re

quire

that

app

ropr

iate

act

ions

are

take

n.

U

nder

perfo

rman

ce ru

les

for t

he O

fLs

will

be e

stab

lishe

d at

a la

ter s

tage

.

Dis

clai

mer

The

EUPT

-Pan

el r

etai

ns th

e rig

ht to

cha

nge

any

parts

of t

his

EUPT

– G

ener

al P

roto

col b

ased

on

new

sci

entif

ic o

r tec

hnic

al in

form

atio

n. A

ny c

hang

es w

ill be

com

mun

icat

ed in

due

cou

rse.

Appendix 9. Specific Protocol of EUPT-SRM13

A-47

A9

Spec

ific

pro

toco

l

Appendix 9 Specific Protocol of EUPT-SRM13

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 1

of 7

SP

ECIF

IC P

ROTO

COL

for t

he 1

3th E

U P

rofic

ienc

y Te

st

on P

estic

ides

requ

iring

Sin

gle

Resi

due

Met

hods

EU

PT –

SRM

13 (2

018)

(r

elea

sed

on 0

9.Ap

ril, 2

018)

Intr

oduc

tion

This

prot

ocol

is c

ompl

emen

tary

to th

e va

lid v

ersio

n of

the

"Gen

eral

Pro

toco

l for

EU

Pro

ficie

ncy

Test

s fo

r Pes

ticid

e Re

si-

dues

in F

ood

and

Feed

" co

verin

g al

l EU

PTs.

Th

e EU

PT-S

RM13

is o

rgan

ised

by t

he E

U R

efer

ence

Lab

orat

ory

for

pest

icid

es r

equi

ring

Sing

le R

esid

ue M

etho

ds (

EURL

– SR

M) w

hich

is a

ccre

dite

d ac

cord

ing

to IS

O 1

7043

as p

rovi

ders

of p

rofic

ienc

y te

sts.

Th

e EU

PT-S

RM13

dea

ls w

ith th

e an

alys

is of

SRM

-pes

ticid

es in

dry

soy

bean

s an

d is

to b

e pe

rfor

med

by

all N

atio

nal R

efer

-en

ce L

abor

ator

ies

for

Sing

le R

esid

ue M

etho

ds (N

RL-S

RMs)

as

wel

l as

by a

ll of

ficia

l EU

labo

rato

ries

(OfL

s) in

volv

ed in

offi

-ci

al p

estic

ide

resid

ue c

ontr

ols

as fa

r as

thei

r sc

ope

over

laps

with

that

of t

he E

UPT

-SRM

13. T

his

incl

udes

labo

rato

ries

in-

volv

ed in

impo

rt c

ontr

ol w

ithin

the

fram

e of

Reg

. 669

/200

9/EC

. A s

peci

al E

UPT

-SRM

13-W

ebsi

te c

onta

inin

g lin

ks t

o th

e m

ost i

mpo

rtan

t doc

umen

ts o

f rel

evan

ce w

as c

onst

ruct

ed.

A pr

elim

inar

y se

lect

ion

of th

e la

bora

torie

s co

nsid

ered

to b

e ob

liged

to p

artic

ipat

e in

the

pres

ent w

as d

one

base

d on

the

info

rmat

ion

in th

e of

ficia

l Lab

-Net

wor

k-da

taba

se h

oste

d in

the

EURL

Dat

aPoo

l and

con

sider

ing

the

com

mod

ity sc

ope

only

(n

ot th

e pe

stic

ide

scop

e). T

he s

tatu

s of

the

OfL

s co

ncer

ning

thei

r par

ticip

atio

n in

the

curr

ent P

T w

as s

how

n on

the

regi

s-tr

atio

n pa

ge. A

s fa

r as

the

EU

PT-S

RM13

is c

once

rned

, all

OfL

s an

alys

ing

pest

icid

es o

f fo

od a

nd f

eed

in t

he c

omm

odity

gr

oup

“hig

h oi

l con

tent

and

ver

y lo

w w

ater

con

tent

” w

ere

cons

ider

ed a

s ob

liged

to

part

icip

ate

in t

his

PT. O

fLs

liste

d as

“o

blig

ed t

o pa

rtic

ipat

e in

the

EU

PT-S

RM13

” bu

t no

t in

tend

ing

to p

artic

ipat

e ha

d to

sta

te t

heir

reas

ons

for

non-

part

icip

atio

n du

ring

the

onlin

e re

gist

ratio

n of

the

EU

PT-S

RM13

, whi

ch la

sted

from

26

Febr

uary

till

16

Mar

ch, 2

018.

The

fe

edba

ck re

ceiv

ed d

urin

g re

gist

ratio

n is

cons

ider

ed in

the

final

list

of o

blig

ed la

bora

torie

s.

Test

Item

and

Bla

nk M

ater

ial

This

EUPT

dea

ls w

ith th

e an

alys

is of

pes

ticid

e re

sidue

s in

Soyb

ean

Flou

r.

Part

icip

ants

will

rece

ive

two

bott

les c

onta

inin

g:

1) c

a. 2

00 g

Tes

t Ite

m w

ith a

sele

ctio

n of

incu

rred

and

spik

ed a

naly

tes f

rom

the

Targ

et P

estic

ides

Lis

t.

2) c

a. 2

00 g

Bla

nk M

ater

ial,

that

can

be

used

for r

ecov

ery

expe

rimen

ts a

s w

ell a

s fo

r th

e pr

epar

atio

n of

mat

rix-

mat

ched

cal

ibra

tion

stan

dard

s

Sp

ecifi

c Pr

otoc

ol |

EU

PT –

SRM

12 (2

017)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 2

of 7

U

sing

rand

omly

cho

sen

bott

les,

the

Org

anize

rs w

ill c

heck

the

Test

Item

for s

uffic

ient

hom

ogen

eity

and

for t

he s

tabi

lity

of

the

pest

icid

es c

onta

ined

ove

r the

per

iod

of th

e ex

erci

se. T

he B

lank

Mat

eria

l will

be

also

che

cked

to p

rove

that

non

e of

the

pest

icid

es o

n th

e Ta

rget

Pes

ticid

es L

ist is

con

tain

ed a

t rel

evan

t lev

els.

Targ

et A

naly

tes a

nd M

RRLs

The

Test

Item

will

con

tain

sev

eral

pes

ticid

es fr

om th

e EU

PT-S

RM13

Tar

get

Pest

icid

es L

ist.

Labo

rato

ries

shou

ld r

ead

this

list c

aref

ully

, as

it sh

ows

how

the

resid

ues

are

expe

cted

to b

e re

port

ed a

s w

ell a

s th

e M

inim

um R

equi

red

Repo

rtin

g Le

v-el

s (M

RRLs

). Th

e M

RRL

valu

es w

ill b

e us

ed to

hel

p id

entif

y fa

lse p

ositi

ve a

nd fa

lse n

egat

ive

resu

lts a

nd fo

r the

cal

cula

tion

of z

-sco

res

for

false

neg

ativ

es. M

ake

sure

to d

ownl

oad

the

late

st v

ersi

on o

f the

EU

PT-S

RM13

Tar

get P

estic

ides

Lis

t be

-fo

re st

artin

g w

ith a

naly

sis a

nd re

sult

repo

rtin

g.

Plea

se n

ote,

the

defin

ition

s of t

he fo

llow

ing

targ

et p

estic

ides

was

mod

ified

:

“Chl

orm

equa

t cat

ion”

and

“m

epiq

uat c

atio

n” w

ere

chan

ged

to “

chlo

rmeq

uat c

hlor

ide”

and

“m

epiq

uat c

hlor

ide”

re

spec

tivel

y, to

refle

ct th

e ne

w w

ordi

ng o

f the

MRL

-reg

ulat

ion

“P

hosp

hane

” w

as c

hang

ed to

“Ph

opha

ne (p

hosp

hine

, inc

l. ph

osph

ane

rele

ased

from

pho

sphi

de s

alts

)”, t

o re

flect

th

e ne

w w

ordi

ng o

f the

MRL

-reg

ulat

ion

It sh

ould

not

be

assu

med

that

onl

y pe

stic

ides

regi

ster

ed fo

r use

in S

oybe

ans a

re p

rese

nt in

the

Test

Item

. Sh

ipm

ent o

f Tes

t Ite

m

Test

item

and

Bla

nk M

ater

ial a

re p

lann

ed to

be

ship

ped

on 2

3 Ap

ril, 2

018.

Co

oled

Tes

t Ite

m a

nd B

lank

Mat

eria

l will

be

pack

ed in

ther

mo-

boxe

s to

geth

er w

ith c

ool g

el p

acks

and

shi

pped

from

Ger

-m

any

via

DHL

expr

ess

parc

el t

o th

e pa

rtic

ipan

ts. P

rior

to s

hipm

ent

a re

min

der

will

be

sent

to th

e pa

rtic

ipat

ing

labo

rato

-rie

s by

e-m

ail.

La

bora

torie

s mus

t mak

e th

eir o

wn

arra

ngem

ents

for t

he re

ceip

t of t

he p

acka

ge. T

hey

shou

ld in

form

the

Org

anise

rs o

f any

pu

blic

hol

iday

s in

the

ir co

untr

y/ci

ty d

urin

g th

e w

eek

of t

he s

hipm

ent,

and

mus

t m

ake

the

nece

ssar

y ar

rang

emen

ts t

o re

ceiv

e th

e sh

ipm

ent,

even

if th

e la

bora

tory

is c

lose

d.

Shou

ld a

ny c

ompl

icat

ions

dur

ing

ship

men

t, de

liver

y or

the

cus

tom

s be

exp

ecte

d, t

he p

artic

ipat

ing

labo

rato

ries

shou

ld

prov

ide

the

Org

anize

rs in

adv

ance

with

con

tact

info

rmat

ion

of p

ossib

le c

onta

ct p

erso

ns o

f th

e la

b (e

.g. m

obile

pho

ne

num

bers

) as

wel

l as

inst

ruct

ions

in lo

cal l

angu

age

expl

aini

ng t

he n

eed

to k

eep

the

pack

age

in f

reez

er d

urin

g de

lay

in

tran

sit a

nd d

eliv

ery.

Thi

s inf

orm

atio

n w

ill b

e at

tach

ed to

the

pack

age.

Af

ter

the

pack

ages

wer

e pi

cked

up

and

stor

ed in

the

DHL

del

iver

y sy

stem

, eac

h pa

rtic

ipan

t w

ill b

e in

form

ed b

y DH

L ab

out t

he tr

acki

ng n

umbe

r of h

is p

acka

ge. T

he p

artic

ipan

ts c

an fo

llow

the

deliv

ery

stat

e of

thei

r ow

n pa

ckag

es o

nlin

e.

Onc

e a

pack

age

has a

rriv

ed th

e re

cipi

ent c

ount

ry a

nd a

n un

expe

cted

del

ay is

not

ices

, the

par

ticip

ant h

imse

lf is

stro

ngly

en

cour

aged

to

cont

act

his

loca

l DHL

Exp

ress

or

the

cust

oms

in o

rder

to

acce

lera

te t

he c

lear

ance

and

del

iver

y pr

oce-

dure

s.


A-48

Appendix 9 (cont.) Specific Protocol of EUPT-SRM13

Spec

ific

Prot

ocol

| E

UPT

– S

RM12

(201

7)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 3

of 7

In

stru

ctio

ns o

n ha

ndlin

g th

e Te

st It

em

Both

Tes

t Ite

m a

nd B

lank

mat

eria

l are

pro

vide

d as

mill

ed fl

our.

Onc

e ar

rived

, the

Tes

t Ite

m s

houl

d be

sto

red

deep

froz

en

(at -

18°C

or l

ower

) unt

il an

alys

is in

ord

er to

avo

id a

ny p

ossib

le d

eter

iora

tion/

spoi

lage

and

to m

inim

ize p

estic

ide

degr

ada-

tion.

Be

fore

ana

lytic

al p

ortio

ns a

re ta

ken

for a

naly

sis, t

he T

est I

tem

sho

uld

be m

ixed

thor

ough

ly in

its

entir

ety.

Dur

ing

mix

ing,

tr

y to

kee

p te

mpe

ratu

res l

ow to

avo

id lo

sses

of s

usce

ptib

le p

estic

ides

. Pa

rtic

ipat

ing

labo

rato

ries

shou

ld u

se th

eir r

outin

e st

anda

rd o

pera

ting

proc

edur

es fo

r ext

ract

ion,

cle

an-u

p an

d an

alyt

i-ca

l mea

sure

men

t as

wel

l as

thei

r ow

n re

fere

nce

stan

dard

s fo

r ide

ntifi

catio

n an

d qu

antif

icat

ion

purp

oses

. Lab

orat

orie

s m

ay a

lso e

mpl

oy m

etho

ds n

ot y

et im

plem

ente

d ro

utin

ely,

for

exa

mpl

e if

they

are

in t

he t

est-

phas

e of

impl

emen

ting

them

. In

this

case

the

limite

d ex

perie

nce

and

the

non-

incl

usio

n of

the

anal

ytes

in th

e ro

utin

e sc

ope

shou

ld b

e in

dica

ted

in

the

EUPT

-SRM

13 R

esul

t Sub

mis

sion

Web

site

. Th

e ho

mog

enei

ty te

sts

will

be

cond

ucte

d us

ing

5 g

for Q

uECh

ERS

and

QuP

Pe a

men

able

pes

ticid

es. A

s su

b-sa

mpl

ing

varia

-bi

lity

incr

ease

s with

dec

reas

ing

anal

ytic

al p

ortio

n siz

e, su

ffici

ent h

omog

enei

ty c

an b

e gu

aran

teed

onl

y fo

r sam

ple

port

ions

eq

ual t

o or

big

ger t

han

the

used

por

tion

size

in th

e ho

mog

enei

ty te

st.

Resu

lts su

bmis

sion

web

site

Sam

ple

rece

ipt a

ckno

wle

dgem

ent,

anal

ytic

al re

sults

and

met

hod

info

rmat

ion

are

to b

e su

bmitt

ed v

ia th

e fo

llow

ing

web

-sit

e: E

UPT

-SRM

13 re

sult

subm

issio

n w

ebsi

te.

Su

b-Pa

ge 0

(Sam

ple

rece

ipt a

ckno

wle

dgem

ent)

, acc

essib

le fr

om 2

5 Ap

ril, 2

018.

Sub-

Page

s 1-3

(ana

lytic

al re

sults

and

met

hod

info

rmat

ion)

acc

essib

le fr

om 3

0 Ap

ril, t

ill 2

2 M

ay, 2

018.

The

dead

line

for r

esul

t sub

miss

ion

is 2

2 M

ay, 2

018

at 1

6 h

(CES

T).

- Log

in C

rede

ntia

l and

Lab

-Cod

e

To a

cces

s th

e da

ta-s

ubm

issi

on f

orm

s pa

rtic

ipan

ts m

ust

use

thei

r un

ique

logi

n cr

eden

tials

(use

rnam

e an

d pa

ssw

ord)

. Th

e lo

gin

cred

entia

l tog

ethe

r with

the

EUPT

-SRM

13 la

b-co

des

will

be

prov

ided

to e

ach

of th

e pa

rtic

ipat

ing

labo

rato

ries

on th

e sh

ipm

ent d

ay.

- Sam

ple

Rece

ipt a

nd A

ccep

tanc

e (S

ub-P

age

0)

Onc

e th

e la

bora

tory

has

rec

eive

d th

e pa

ckag

e it

mus

t re

port

to

the

orga

nise

r vi

a th

e EU

PT-S

RM13

Res

ult

Subm

issi

on

Web

site

(sub

-pag

e 0)

the

date

of r

ecei

pt, t

he c

ondi

tion

of th

e Te

st It

em, a

nd it

s ac

cept

ance

. For

labo

rato

ries

in th

e EU

- an

d EF

TA c

ount

ries

and

EU c

andi

date

cou

ntrie

s, th

e de

adlin

e fo

r ac

cept

ance

is 2

7 Ap

ril, 2

018.

If a

labo

rato

ry d

oes

not

resp

ond

by th

is de

adlin

e, th

e O

rgan

isers

will

ass

ume

that

Tes

t Ite

m a

nd B

lank

Mat

eria

l hav

e be

en re

ceiv

ed a

nd a

ccep

ted.

An

y pa

rtici

pant

s th

at h

ave

not r

ecei

ved

the

Test

Item

s by

the

27 A

pril

at n

oon,

they

mus

t inf

orm

the

Org

anise

r vi

a e-

mai

l (E

URL-

SRM

@cv

uas.b

wl.d

e). T

he O

rgan

iser w

ill c

onsu

lt th

e sh

ippi

ng c

ompa

ny to

loca

lize

the

pack

age

and

decid

e on

furt

her

actio

ns in

cludi

ng n

ew sh

ipm

ent,

if ne

cess

ary.

Sp

ecifi

c Pr

otoc

ol |

EU

PT –

SRM

12 (2

017)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 4

of 7

- R

epor

ting

qual

itativ

e an

d qu

antit

ativ

e Re

sults

(Sub

-Pag

e 1

and

2)

To re

port

thei

r res

ults

, lab

orat

orie

s mus

t acc

ess t

he E

UPT

-SRM

13 R

esul

t Sub

mis

sion

Web

site

. Al

l res

ults

mus

t be

repo

rted

on

this

web

site

by 2

2 M

ay, 2

018

at 1

6 h

(CES

T). T

he w

ebsit

e w

ill n

ot b

e ac

cess

ible

afte

r thi

s de

adlin

e, a

nd a

ll re

sults

subm

itted

afte

rwar

ds w

ill n

ot b

e ac

cept

ed.

Befo

re e

nter

ing

the

resu

lts, p

leas

e st

udy

the

Targ

et P

estic

ide

List

car

eful

ly, i

n pa

rtic

ular

the

res

idue

def

initi

ons

that

ap

ply

to th

e EU

PT, w

hich

are

not

nec

essa

rily

give

n in

full

on th

e Re

sult

Subm

issio

n W

ebsi

te.

The

follo

win

g fie

lds w

ill b

e av

aila

ble

for r

epor

ting

the

quan

titat

ive

resu

lts:

-

“Con

cent

ratio

n in

mg/

kg”:

the

pest

icid

e co

ncen

trat

ions

that

wou

ld b

e re

port

ed in

rout

ine

wor

k. R

esul

ts s

houl

d no

t be

rep

orte

d w

here

a p

estic

ide

was

not

det

ecte

d, o

r w

as d

etec

ted

belo

w th

e RL

(Rep

ortin

g Li

mit)

of t

he la

-bo

rato

ry o

r the

MRR

L. R

esul

ts re

port

ed a

s “<

RL”

or “

< #,

# m

g/kg

” w

ill b

e co

nsid

ered

as „

Not

Det

ecte

d”.

The

resid

ue le

vels

of th

e pe

stic

ides

mus

t be

repo

rted

in m

g/kg

usin

g th

e fo

llow

ing

sign

ifica

nt fi

gure

s:

Le

vels

<0.0

10 m

g/kg

to b

e ex

pres

sed

to 2

sign

ifica

nt fi

gure

s, e

.g. 0

.005

8 m

g/kg

;

Leve

ls ≥

0.01

0 m

g/kg

to b

e ex

pres

sed

to 3

sign

ifica

nt fi

gure

s, e

.g. 0

.156

, 1.6

4, 1

0.3

mg/

kg

Reco

very

-cor

rect

ed r

esul

ts s

houl

d be

rep

orte

d on

ly w

here

thi

s re

flect

s th

e ro

utin

e la

b’s

proc

edur

e; o

ther

wis

e th

e no

n-re

cove

ry-c

orre

cted

res

ult

shou

ld b

e re

port

ed.

Whe

re a

res

ult

was

cor

rect

ed f

or r

ecov

ery

the

ap-

proa

ch(e

s) fo

llow

ed to

ach

ieve

this

corr

ectio

n (e

.g. s

tand

ard

addi

tions

to sa

mpl

e po

rtio

ns, p

roce

dura

l cal

ibra

tion,

re

cove

ry m

ust b

e re

port

ed in

the

resp

ectiv

e fie

lds

in S

ubpa

ge 3

fact

or, u

se o

f ILI

S).

-

“Con

c. in

bla

nk in

mg/

kg”:

con

cent

ratio

n va

lues

of a

ny p

estic

ides

from

the

Targ

et P

estic

ide

List

det

erm

ined

in

the

Blan

k M

ater

ial (

even

at l

evel

s bel

ow th

e M

RRL)

. -

“Exp

erie

nce

with

this

com

poun

d”: U

se th

e dr

opdo

wn-

men

u to

indi

cate

for h

ow m

any

year

s you

hav

e be

en a

na-

lysin

g fo

r eac

h co

mpo

und

usin

g th

e m

etho

d ap

plie

d in

this

EUPT

.

- Rep

ortin

g In

form

atio

n on

Ana

lytic

al M

etho

dolo

gy (S

ub-P

age

3)

On

sub-

page

3 o

f the

“EU

PT-S

RM13

Res

ult S

ubm

issi

on W

ebsi

te”

the

part

icip

atin

g la

bora

torie

s m

ust p

rovi

de C

OM

PLET

E in

form

atio

n on

the

ana

lytic

al m

etho

d(s)

app

lied

to a

ll pe

stic

ides

whi

ch w

ere

anal

ysed

, irr

espe

ctiv

e of

whe

ther

the

y w

ere

dete

cted

or n

ot.

The

part

icip

atin

g la

bora

torie

s ar

e ur

ged

to th

orou

ghly

fill-

in a

ll re

ques

ted

info

rmat

ion

and

cont

rol i

t car

eful

ly in

ord

er to

m

inim

ize

the

adm

inist

rativ

e bu

rden

of c

olle

ctin

g an

d co

rrec

ting

it a

post

erio

ri.

If no

suf

ficie

nt in

form

atio

n on

the

met

hodo

logy

use

d is

pro

vide

d, t

he O

rgan

iser

s re

serv

e th

e rig

ht n

ot t

o ac

cept

the

an

alyt

ical

resu

lts re

port

ed b

y th

e pa

rtic

ipan

t or t

o re

fuse

par

ticip

atio

n is

futu

re E

UPT

-SRM

s.

For

deta

iled

info

rmat

ion

on

the

colu

mns

on

su

b-pa

ge

3 pl

ease

re

fer

to

the

Guid

e on

Re

sult

Subm

issio

n (h

ttp:

//w

ww

.eur

l-pes

ticid

es.e

u/lib

rary

/doc

s/sr

m/E

UPT

-SRM

13_S

hort

_Gui

de_S

ubPa

ges.

pdf).

O

nce

your

re

sults

ar

e co

mpl

etel

y su

bmitt

ed, p

leas

e ex

port

them

via

the

func

tion

on th

e su

bmis

sion

Mai

n Pa

ge a

s a

csv-

form

at. T

his

file

can

be v

iew

ed v

ia E

xcel

, and

you

can

eas

ily c

heck

you

r ent

ries s

tore

d in

the

data

base

.

Appendix 9. Specific Protocol of EUPT-SRM13

A-49


A9

Spec

ific

pro

toco

l

Sp

ecifi

c Pr

otoc

ol |

EU

PT –

SRM

12 (2

017)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 5

of 7

Su

bcon

trac

ting

The

follo

win

g ta

sk w

as su

bcon

trac

ted

to th

e EU

RL-C

F, S

øbor

g, D

enm

ark:

a)

Gene

ratio

n of

the

logi

n cr

eden

tials

b)

Adm

inist

ratio

n of

EU

PT-S

RM13

resu

lt su

bmiss

ion

web

site

Follo

w-u

p ac

tions

Afte

r the

dist

ribut

ion

of th

e EU

PT-S

RM13

Pre

limin

ary

Repo

rt, l

abor

ator

ies

with

poo

r res

ults

(hig

h ab

solu

te z

-sco

res,

false

ne

gativ

es o

r fa

lse p

ositi

ves)

will

be

aske

d to

pro

vide

info

rmat

ion

conc

erni

ng th

e re

ason

s fo

r th

is an

d po

ssib

le c

orre

ctiv

e ac

tions

. Thi

s in

form

atio

n w

ill b

e fo

rwar

ded

to t

he c

orre

spon

ding

NRL

-SRM

s up

on r

eque

st. A

ll EU

PT-S

RM13

-par

ticip

ants

ar

e w

elco

me

to a

sk th

e EU

RL-S

RM fo

r tec

hnic

al a

ssist

ance

. Th

e O

rgan

iser

mig

ht a

sk la

bora

torie

s to

pro

vide

miss

ing

met

hodo

logy

info

rmat

ion

that

is im

port

ant

for

the

eval

uatio

n an

d in

terp

reta

tion

of th

e PT

. Ac

cord

ing

to in

stru

ctio

ns b

y DG

-SAN

TE,

the

“Pro

toco

l for

man

agem

ent

of u

nder

perf

orm

ance

in c

ompa

rativ

e te

stin

g an

d/or

lack

of c

olla

bora

tion

of N

atio

nal R

efer

ence

Lab

orat

orie

s (N

RLs)

with

Com

mun

ity r

efer

ence

labo

rato

ries

(CRL

s)

activ

ities

” w

ill b

e fo

llow

ed b

y N

RLs.

Do

cum

ents

All d

ocum

ents

rela

ted

to th

e EU

PT–S

RM13

can

be

foun

d in

the

EURL

-Doc

umen

t Rep

osito

ry (C

IRCA

-BC)

. Lin

ks to

the

doc-

umen

ts c

an a

lso b

e fo

und

in th

e EU

PT-S

RM13

Web

site

. Fo

r fur

ther

info

rmat

ion

plea

se c

onta

ct th

e or

gani

zers

EU

RL-S

RM@

cvua

s.bw

l.de

Plea

se c

heck

the

EUPT

-SRM

13 W

ebsi

te b

efor

e st

artin

g w

ith th

e an

alys

is to

mak

e su

re th

at y

ou h

ave

the

late

st v

ersi

on o

f al

l doc

umen

ts a

vaila

ble.

In c

ase

of m

ajor

cha

nges

the

part

icip

ants

will

be

info

rmed

via

e-m

ail.

Part

icip

atio

n fe

es a

nd p

aym

ent d

etai

ls

To c

over

the

cos

ts o

f pro

duct

ion,

han

dlin

g an

d sh

ipm

ent

of t

he P

T-M

ater

ials

the

follo

win

g fe

es w

ill b

e ch

arge

d fo

r on

e un

it of

the

PT-M

ater

ial t

o th

e pa

rtic

ipat

ing

labo

rato

ries:

- OfL

s (in

clud

ing

NRL

s) fr

om E

U c

ount

ries,

EU-c

andi

date

cou

ntrie

s and

EFT

A co

untr

ies:

200

€

- Lab

s bas

ed in

third

cou

ntrie

s: 3

50 €

An

invo

ice

issu

ed t

o th

e "i

nvoi

ce a

ddre

ss"

stat

ed in

the

reg

istr

atio

n fo

rm w

ill b

e se

nt t

o th

e in

voic

e e-

mai

l add

ress

st

ated

dur

ing

regi

stra

tion.

Sho

uld

the

paym

ent b

eing

take

n ca

re o

f by

anot

her d

epar

tmen

t/in

stitu

tion,

the

reci

pien

t of

the

invo

ice

is re

ques

ted

to fo

rwar

d th

e in

voic

e ac

cord

ingl

y. D

etai

ls o

f pay

men

t will

be

give

n in

the

invo

ices

. Pa

ymen

t is

expe

cted

to b

e m

ade

with

in 3

0 da

ys u

pon

the

date

of s

hipm

ent

unle

ss s

peci

al in

form

atio

n w

as p

rovi

ded

by

the

part

icip

ant d

urin

g re

gist

ratio

n an

d/or

oth

erw

ise a

gree

d be

twee

n pa

rtic

ipan

t and

org

anise

r.

If fo

r any

reas

on p

aym

ent c

anno

t be

carr

ied

out b

efor

e th

is d

ate,

ple

ase

cont

act t

he O

rgan

izer t

o gi

ve e

xpla

natio

ns.

If no

pay

men

t or n

o pr

oof o

f pay

men

t is

rece

ived

and

no

expl

anat

ion

is g

iven

to th

e O

rgan

izers

, the

Org

anize

rs re

serv

e

Sp

ecifi

c Pr

otoc

ol |

EU

PT –

SRM

12 (2

017)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 6

of 7

th

e rig

ht to

exc

lude

the

resu

lts o

f the

con

cern

ed la

bora

torie

s fr

om th

e Fi

nal E

UPT

-Rep

ort o

r to

refu

se it

s pa

rtic

ipat

ion

in fu

ture

EU

PT-S

RMs.

Ba

nk D

etai

ls:

Bank

acc

ount

hol

der:

La

ndes

ober

kass

e Ba

den

Wue

rtte

mbe

rg

Bank

Nam

e :

Bade

n W

uert

tem

berg

isch

e Ba

nk

IBAN

: DE

02

6005

010

1 74

95 5

301

02

BIC/

SWIF

T:

SOLA

DEST

XXX

Paye

e id

entif

icat

ion

text

:

VAT

of C

VUA

Stut

tgar

t Se

e in

voic

e (im

port

ant a

nd M

UST

be

indi

cate

d!)

DE 8

11 6

00 5

10

To fa

cilit

ate

trac

king

of m

oney

tran

sfer

the

spec

ial p

ayee

iden

tific

atio

n te

xt (=

invo

ice

num

ber)

as

show

n in

the

invo

ice

MU

ST b

e in

dica

ted

in th

e re

mitt

ance

. M

ore

deta

ils fo

r ban

k-re

mitt

ance

are

giv

en in

the

invo

ices

. Ca

lend

ar o

f EU

PT-S

RM13

(p

leas

e se

e ht

tp:/

/ww

w.e

url-p

estic

ides

.eu/

libra

ry/d

ocs/

srm

/EU

PT-S

RM13

_Cal

enda

r.pdf

)

Targ

et P

estic

ides

List

of E

UPT

-SRM

13

(ple

ase

see

http

://w

ww

.eur

l-pes

ticid

es.e

u/lib

rary

/doc

s/sr

m/E

UPT

-SRM

13_T

arge

tPes

ticid

eList

.pdf

)


A-50


Spec

ific

Prot

ocol

| E

UPT

– S

RM12

(201

7)

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) CV

UA

Stut

tgar

t, Sc

hafla

ndst

r. 3/

2, D

E-70

736

Fellb

ach

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 7

of 7

Co

ntac

t inf

orm

atio

n

EU R

efer

ence

Lab

orat

ory

for S

ingl

e Re

sidu

e M

etho

ds (E

URL

-SRM

) Ch

emisc

hes u

nd V

eter

inär

unte

rsuc

huns

amt S

tutt

gart

Sc

hafla

ndst

r. 3/

2,

D-

7073

6 Fe

llbac

h

Germ

any

e-m

ail:

EURL

-SRM

@cv

uas.

bwl.d

e

Fax:

+49

342

6 11

24

Org

anis

ing

Gro

up a

t the

EU

RL-S

RM (S

tutt

gart

)

Mic

hela

ngel

o An

asta

ssia

des

phon

e: +

49 3

426

1124

Pa

t Sch

reite

r ph

one:

+49

342

6 10

29

Carm

en W

ausc

hkuh

n

phon

e: +

49 3

426

1159

Hu

bert

Zip

per

phon

e: +

49 3

426

1141

An

ja B

arth

ph

one:

+49

342

6 19

35

Giov

anna

Cer

chia

ph

one:

+49

342

6 11

14

Advi

sory

Gro

up

Amad

eo F

erná

ndez

-Alb

a EU

RL-F

V, U

nive

rsity

of A

lmer

ía (U

AL),

ES

Mig

uel G

amón

EU

RL-F

V, L

abor

ator

io A

groa

limen

tario

Gen

eral

itat V

alen

cian

a (L

AGV)

, ES

Met

te E

reci

us P

oulse

n EU

RL-C

F, N

atio

nal F

ood

Inst

itute

(DTU

), Sø

borg

, DK

Ralf

Lipp

old

EURL

-AO

, CVU

A Fr

eibu

rg, D

E Ph

ilipp

e Gr

os

Serv

ice

Com

mun

des

Lab

orat

oire

s (SC

L) /

Labo

rato

ire d

e M

ontp

ellie

r, FR

M

agnu

s Jez

usse

k Ba

varia

n He

alth

and

Foo

d Sa

fety

Aut

horit

y (L

GL),

Erla

ngen

, DE

Andr

é de

Kok

N

ethe

rland

s Foo

d an

d Co

nsum

er P

rodu

ct S

afet

y Au

thor

ity (N

VWA)

, Am

ster

dam

, NL

Sonj

a M

asse

lter

Aust

rian

Agen

cy fo

r Hea

lth a

nd F

ood

Safe

ty (A

GES)

, Inn

sbru

ck, A

T

Finb

arr O

’Reg

an

Pest

icide

Con

trol

Labo

rato

ry (P

CL),

Dept

. of A

gricu

lture

, Foo

d an

d th

e M

arin

e (D

AFM

) IR

Tuija

Pih

lströ

m

Swed

ish N

atio

nal F

ood

Agen

cy (S

NFA

-Liv

smed

elsv

erke

t), U

ppsa

la, S

E Ca

rmel

o Ro

dríg

uez

Uni

vers

ity o

f Alm

ería

(UAL

), Sp

ain

Qua

lity

Cont

rol G

roup

Anto

nio

Valv

erde

Uni

vers

ity o

f Alm

ería

(UAL

), ES

Pa

ula

Med

ina

Euro

pean

Foo

d Sa

fety

Aut

horit

y (E

FSA)

Appendix 10. Calendar and Target Pesticides List of EUPT-SRM13

A-51

Cale

nd

ar a

nd

T a

rgeT

Pes

TiCi

de l

isT

a10

EU R

efer

ence

Lab

orat

ory

Requ

iring

Sin

gle

Resi

due

Met

hods

(EU

RL-S

RM)

CVU

A St

uttg

art,

Scha

fland

str.

3/2,

DE-

7073

6 Fe

llbac

h, G

erm

any

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

eurl-

srm

@cv

uas.

bwl.d

e Pa

ge 1

of 1

TARG

ET P

ESTI

CIDE

LIST

fo

r the

EU

PT –

SRM

13 2

018,

Dry

Soy

bean

s up

date

on

14.0

3.20

18

Com

poun

ds P

oten

tially

Pre

sent

in T

est I

tem

Li

sted

in

MRR

L (m

g/kg

)

Com

puls

ory

Com

poun

ds (w

ill b

e co

nsid

ered

in C

ateg

ory

A/B

clas

sific

atio

n)

2,4-

D (fr

ee a

cid,

no

hydr

olys

is st

ep to

be

appl

ied)

M

ACP-

Reg.

0.

01

Brom

ide

ion

MAC

P-Re

g.

2

Chlo

rmeq

uat c

hlor

ide

MAC

P-Re

g.

0.01

Cyro

maz

ine

MAC

P-Re

g.

0.01

Ethe

phon

M

ACP-

Reg.

0.

02

Flua

zifo

p (fr

ee a

cid,

no

hydr

olys

is st

ep to

be

appl

ied)

M

ACP-

Reg.

0.

01

Gly

phos

ate

(par

ent o

nly)

M

ACP-

Reg.

0.

03

Halo

xyfo

p (fr

ee a

cid,

no

hydr

olys

is st

ep to

be

appl

ied)

M

ACP-

Reg.

0.

003

Mep

iqua

t chl

orid

e

MAC

P-Re

g.

0.01

Opt

iona

l Com

poun

ds (w

ill N

OT

be c

onsi

dere

d in

Cat

egor

y A/

B cl

assi

ficat

ion)

2,4-

DB (f

ree

acid

, no

hydr

olys

is st

ep to

be

appl

ied)

N

CP-W

D 0.

01

Bent

azon

e (fr

ee a

cid,

no

hydr

olys

is st

ep to

be

appl

ied)

–

0.02

Carb

ofur

an (s

um, e

xcep

t 3-O

H-CF

) M

ACP-

Reg.

0.

005

Chlo

rate

(ani

on)

NCP

-WD

0.01

Diqu

at (d

icat

ion)

N

CP-W

D 0.

02

Feno

xapr

op (f

ree

acid

, no

hydr

olys

is st

ep to

be

appl

ied)

–

0.01

Glu

fosi

nate

N

CP-W

D 0.

02

MPP

(met

abol

ite o

f glu

fosi

nate

) N

CP-W

D 0.

02

N-A

cety

l-Glu

fosi

nate

(met

abol

ite o

f glu

fosi

nate

) N

CP-W

D 0.

02

AMPA

(met

abol

ite o

f gly

phos

ate)

N

CP-W

D 0.

05

N-A

cety

l-Gly

phos

ate

(met

abol

ite o

f gly

phos

ate)

N

CP-W

D 0.

02

Para

quat

(dic

atio

n)

NCP

-WD

0.02

Perc

hlor

ate

(ani

on)

Cont

amin

ant

0.01

Phos

phan

e (p

hosp

hine

, inc

l. Ph

osph

ane

rele

ased

from

pho

sphi

de sa

lts)

NCP

-WD

0.00

5

Phos

phon

ic a

cid

NCP

-WD

0.05

Qui

zalo

fop

(free

aci

d, n

o hy

drol

ysis

step

to b

e ap

plie

d)

NCP

-WD

0.01

MAC

P-Re

g.: M

ACP

Regu

latio

n

NCP

-WD:

Wor

king

Doc

umen

t SAN

CO/1

2745

/201

3, 2

1 –2

2 N

ovem

ber 2

017

rev.

9(1

)

Not

e: T

his

docu

men

t may

be

subj

ect t

o m

inor

cha

nges

. In

case

of s

igni

fican

t cha

nges

the

orga

nize

rs w

ill s

end

e-m

ails

. In

any

case

ple

ase

chec

k ou

r web

site

perio

dica

lly to

mak

e su

re y

ou a

re u

sing

the

late

st a

vaila

ble

vers

ion.

For a

ny fu

rthe

r cla

rific

atio

n do

n’t h

esita

te to

con

tact

us u

nder

eur

l-srm

@cv

uas.

bwl.d

e

The

EUPT

-SRM

13 O

rgan

isin

g Te

am

Appendix 10 Calendar and Target Pesticides List of EUPT-SRM13

EU R

efer

ence

Lab

orat

ory

Requ

iring

Sin

gle

Resi

due

Met

hods

(EU

RL-S

RM)

CVU

A St

uttg

art,

Scha

fland

str.

3/2,

DE-

7073

6 Fe

llbac

h, G

erm

any

Web

site:

ww

w.e

url-p

estic

ides

.eu,

E-M

ail:

EURL

-SRM

@cv

uas.

bwl.d

e Pa

ge 1

of 1

CC AALL EE

NNDD

AARR

ff oorr tt

hh ee EE

UUPP TT

–– SS

RR MM11 33

So

ybea

ns

(rel

ease

d on

23

Janu

ary,

201

8)

Activ

ity

Who

? Da

tes

Ope

ning

of t

he E

UPT

-SRM

13 W

ebsi

te

with

link

s to

all r

elev

ant d

ocum

ents

(C

alen

dar,

Targ

et P

estic

ides

Lis

t, G

ener

al P

roto

col)

EURL

-SRM

23

Jan.

, 201

8

Regi

stra

tion

via

“EU

PT-R

egis

trat

ion

Web

site

”

(Not

e: O

blig

ed L

abor

ator

ies M

UST

ent

er th

is W

ebsit

e an

d ei

ther

regi

s-te

r or g

ive

expl

anat

ions

for n

on-p

artic

ipat

ion)

All L

abor

ator

ies i

nter

este

d in

par

ticip

atio

n an

d al

l ob

liged

labs

eve

n if

not

inte

rest

ed

26 F

eb. –

16

Mar

ch 2

018

Disp

atch

of E

UPT

-SRM

13-S

peci

fic P

roto

col

EURL

-SRM

Ap

ril 2

018

Prep

arat

ion

of E

UPT

-SRM

13-T

est I

tem

(p

relim

inar

y te

sts S

piki

ng /

Hom

ogen

izatio

n)

EURL

-SRM

M

arch

201

8 –

April

201

8

Hom

ogen

eity

Tes

ts

EURL

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M

arch

201

8 –

April

201

8

Stab

ility

Tes

ts

EURL

-SRM

Ap

ril –

June

201

8

Ship

men

t of E

UPT

-SRM

13 T

est I

tem

(+

rem

inde

r of u

pcom

ing

parc

el a

rriv

al)

EURL

-SRM

23

Apr

il, 2

018

Conf

irmat

ion

of sa

mpl

e Re

ceip

t and

acc

epta

nce

via

“EU

PT-S

RM13

Res

ult S

ubm

issi

on W

ebsi

te",

(S

ub-P

age

0)

Part

icip

atin

g La

bs

with

in 4

8 h

of re

ceip

t

Resu

lt Su

bmis

sion

(P

estic

ide

scop

e, R

esul

ts, M

etho

d In

fo) i

n

“EU

PT-S

RM13

Res

ult S

ubm

issi

on W

ebsi

te",

(S

ub-P

ages

1 –

3)

Part

icip

atin

g La

bs

30 A

pril

– 22

May

201

8

Prel

imin

ary

Repo

rt

(onl

y co

mpi

latio

n of

resu

lts a

nd p

relim

inar

y as

signe

d va

lues

) EU

RL-S

RM

June

201

8

EUPT

Eva

luat

ion

Mee

ting

EUPT

-SC,

DG-

SAN

TE

–

Surv

ey to

col

lect

reas

ons f

or u

nder

perf

orm

ance

an

d m

issin

g in

form

atio

n on

met

hods

EU

RL-S

RM /

Pa

rtic

ipat

ing

Labs

Ju

ne /

July

201

8

Fina

l Rep

ort

EURL

-SRM

De

c. 2

018

REM

ARK:

Ple

ase

note

that

the

date

s men

tione

d ab

ove

may

be

subj

ect t

o m

inor

cha

nges

. In

the

case

of c

hang

es th

e pa

r-tic

ipan

ts w

ill b

e in

form

ed v

ia e

-mai

l. Bu

t ple

ase,

still

che

ck p

erio

dica

lly o

ur w

ebsi

te fo

r pos

sible

upd

ates

in c

ase

the

emai

l doe

s not

get

thro

ugh

to y

ou.

Cont

act:

eurl-

srm

@cv

uas.

bwl.d

e

The

EUPT

-SRM

Tea

m

European Union Reference Laboratory for pesticides requiring Single Residue Methods (EURL – SRM) hosted at Chemisches Veterinäruntersuchungsamt Stuttgart (CVUA Stuttgart)

Schaflandstr. 3/2 70736 Fellbach Germany Tel: + 49 711 3426 1124Fax: + 49 711 58 81 76

http://www.srm.eurl-pesticides.eue-mail: [email protected]

eurl-srm eu reference laboratories for residues of ...€¦ · introduction ix ntrodu c t on...

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