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EUROPEAN UNION PROFICIENCY TEST FOR PESTICIDES IN FRUIT AND VEGETABLES.

SCREENING METHODS 04 (EUPT-FV-SM-04)

2012

Pesticide Residues in Pear Homogenate

Final Report Organiser:

Dr. Amadeo R. Fernández-Alba Co-Head of EURL-FV

University of Almería, Edificio Químicas CITE I, Ctra. Sacramento s/n 04120 Almería, SPAIN

Phone: +34 950015034; Fax: +34 950015645 E-mail: [email protected] www.eurl-pesticides.eu

Organising team at the University of Almería:

Dr. Paula Medina, Chemist. University of Almería Mr. Octavio Malato, Chemist. University of Almería Ms. Carmen Ferrer, Chemist. University of Almería Ms. Noelia Belmonte, Chemist. University of Almería Ms. Ana Lozano, Chemist. University of Almería Ms. Mª del Mar Gómez, Chemist. University of Almería Ms. Samanta Uclés, Chemist. University of Almería Ms. Ana Uclés, Chemist. University of Almería

Quality Control Group

Dr. Antonio Valverde, Senior Chemist, University of Almería, Spain.

Mr. Stewart Reynolds, Senior Chemist, FERA, York, United Kingdom.

Statistical Group

Dr. Carmelo Rodriguez, Senior Mathematician, University of Almeria, Spain.

Advisory Group

Dr. André de Kok, Senior Chemist, NVWA, Wageningen, The Netherlands. Dr. Tuija Pihlström, Senior Chemist NFA, Uppsala, Sweden. Dr. Sonja Masselter, Senior Chemist, AGES, Innsbruck, Austria. Dr. Darinka Stajnbaher, Senior Chemist, IPH, Maribor, Slovenia. Dr. Magnus Jezussek, Senior Chemist, LGL, Erlangen, Germany. Dr. Miguel Gamón, Senior Chemist, Lab. Agroalimentario, Valencia, Spain. Dr. Mette Erecius Poulsen, Senior Chemist, DTU, Copenhagen, Denmark. Mr. Ralf Lippold, Senior Chemist, CVUA, Freiburg, Germany. Dr. Michelangelo Anastassiades, Senior Chemist, CVUA, Stuttgart, Germany.

CONTENTS

1. INTRODUCTION. 1

2. TEST MATERIALS. 2

2.1 Test material.

2.2 Analytical methods.

2.3 Prior analysis of the spiked pear test material.

2.4 Distribution of test material and protocol to participants.

3. STATISTICAL METHODS. 6

3.1 Type of Results Reported.

4. RESULTS. 7

4.1 Summary of reported results.

4.2 Concentration levels.

4.3 Assessment of laboratory performance.

5. CONCLUSIONS. 13

6. SUGGESTIONS FOR FUTURE WORK. 14

7. REFERENCES. 15

8. ACKNOWLEDGEMENTS. 16

APPENDIX 1. Results. 17

APPENDIX 2. Graphical Representations. 19

APPENDIX 3. Methods used by participants for detecting pesticides. 23 (available only as a pdf document uploaded to the EUPT-SM04 webpage, not in the printed version).

ANNEX 1. List of laboratories that participate in EUPT-FV-SM-04. 103

ANNEX 2. Specific Protocol. 105 (available only as a pdf document uploaded to the EUPT-SM04 webpage, not in the printed version).

EUROPEAN UNION PROFICIENCY TEST FOR PESTICIDES IN FRUITS AND VEGETABLES.

SCREENING METHODS 04 BACKGROUND

According to Article 28 of Regulation 396/2005/EC of the European Parliament and European

Council regarding maximum residue levels for pesticides in, or on, food and feed of plant and

animal origin1: all laboratories analysing samples for the official control of pesticide residues shall

participate in the European Union Proficiency Tests (EUPTs) for pesticide residues, facilitated by

the Commission. These proficiency tests are carried out on an annual basis in order to ensure the

quality, accuracy and comparability of the residue data reported by EU Member States to the

European Commission, as well as by other Member States within the framework of coordinated

national monitoring and surveillance programmes.

Regulation (EC) No 882/20042 lays down the general tasks, duties and requirements of European

Union Reference Laboratories (EURLs) for Food, Feed and Animal Health. Among these tasks is the

provision for independently-organised comparative tests. This is the fourth time that the EURL for

pesticides in fruit and vegetables at the University of Almería, Spain3 has organised a proficiency

test on qualitative screening methods for pesticides in fruit and vegetable commodities.

The aim of these tests is to evaluate laboratory capability when using wide-scope qualitative

and/or semi-quantitative screening methods during routine analysis, for detecting and identifying

unexpected pesticides at levels at, or above 0.01 mg/kg – included in and/or in addition to the

laboratories’ quantitative methods used for frequently-detected pesticides. A second aim is to

encourage official laboratories to extend the scope of their methods in a cost-effective way, by

using the different MS instruments/software and methods available (whether they be old or new).

Participation in this PT remains on a voluntary basis. Besides this, official laboratories have a

significant number of mandatory PTs annually given that the EURL-FV already organises the PT for

quantitative multi-residue pesticide analysis (EUPT-FV14), organised over the same time period.

Nevertheless, all FV-NRLs and FV-Official laboratories involved in the determination of pesticide

residues in fruit and vegetables for the EU-coordinated monitoring programme, or for their own

national programmes, were invited to take part.

This report will be presented to the European Commission Standing Committee for Animal Health

and the Food Chain. Furthermore, DG-SANCO has full access to all EUPT data including the

individual lab-codes/lab-name keys.

1 Regulation (EC) No 396/2005, published in the OJ of the EU L70 of 16.03.2005, as last amended by Regulation 839/2008 published in the OJ of the EU L234 of 30.08.2008. 2 Regulation (EC) No 882/2004 of the European Parliament and of the Council on official controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules. Published in the OJ of the EU L191 of 28.05.2004 3 Commission Regulation (EC) No 776/2006 of 23 May 2006 - amending Annex VII of Regulation (EC) No 882/2004 of the European Parliament and of the Council as regards Community Reference Laboratories.

Final Report - EURL-FV-SM-04, 2012 1

1. INTRODUCTION

In this fourth year, consolidation of inter-laboratory tests for pesticide screening methods among

laboratories seems to be assured; and are even requested by those laboratories not performing

routine analysis on fruit and vegetables. Responding to this demand, the EURL-FV has decided to

continue its operation. The support given by DG SANCO for these methods has greatly assisted

laboratory acceptance by allowing laboratories to conduct screening methods on the EU-

Coordinated Multiannual Programme samples.

Over recent years, it has been observed that many laboratories not only use a full-scan

approach to perform screening but that some also employ modern tandem-mass spectrometers,

even if their sensitivity has to be reduced.

Mass spectrometry plays an essential role in the everyday work carried out by laboratories.

Technological improvements in modern MS systems offer new possibilities for greatly increasing

the scope of MRM analysis. Whereas full-scan measurements are theoretically the best approach

for MS screening, developments in targeted measurements also offer the potential for a

substantially increased scope of analysis. Another reason for conducting this proficiency test on

screening methods is to gather information from laboratories as to the type of software they use

for processing data: whether laboratories are using commercial software and databases or

whether they are internally constructed and search manually. This type of test provides an

overview of such information as well as valuable insight into the possible need for further software

development in the near future.

The aim of the EURL-FV is for laboratories to be able to use mass-spectrometry-based screening

methods routinely, following validation. This is in line with Document N° SANCO/12495/2011 (which

supersedes Document No. SANCO/10684/2009)-Method validation and quality control

procedures for pesticide residues analysis in food and feed.

Only qualitative information was requested for those pesticides detected. It was decided, as in

previous PTs, not to provide the laboratories with a Target Pesticide List so that their capability in

detecting whatever pesticides were present was also evaluated.

Regulation (EC) No 882/2004 lays down the general tasks, duties and requirements for EURLs in

Food, Feed and Animal Health. Amongst these tasks is the provision for independently-organised

comparative tests. The EURL for pesticides in Fruit and Vegetables at the University of Almería,

Spain, has organised the proficiency test on qualitative screening methods for pesticides in fruit/

vegetable commodities. This EUPT-FV-SM04 is aimed at all National Reference Laboratories (NRLs)

and all Official Laboratories (OfLs) for fruit and vegetables in EU Member States. Laboratories

outside this EURL/NRL/OfL-Network were also able to participate on a case-by-case basis,

following consultation with DG SANCO.

2 Final Report - EURL-FV-SM-04, 2012

2. TEST MATERIALS

2.1 Test material

This proficiency test is based on the pesticide-residue analysis of pears. The pears were grown in

Aragón, Spain.

The pesticide treatments were carried out post-harvest using either commercial formulation in

micro-spray solutions or using standard solutions. The test material was frozen (using liquid

nitrogen), chopped, homogenised and sub-sampled into polyethylene bottles that had

previously been coded.

Ten of these bottles containing the test material were chosen randomly and analysed to check

for homogeneity.

The test material was stored frozen (–20ºC) prior to shipment to participants.

Two bottles, again chosen randomly, were analysed over a period of time to confirm the stability

of the pesticides in the test material (firstly, when the test materials were shipped, and then a few

days after the deadline for receipt of participants´ results). There was a further analysis during this

period reproducing the sample shipment i.e. maintaining the sample at room temperature for a

few days to see if there was any degradation of any of the pesticides present in the test material.

These results were not included in the statistical analysis of the proficiency test. The aim was solely

to check pesticide stability during the shipping process and for the duration of the proficiency

test.

Blank material without spiked pesticides was also prepared and shipped for confirmation

purposes.

The pesticides used to spike the pear test material were decided upon by the Quality Control

Group. It was decided that a target pesticide list would not be provided to participants. The

pesticides selected for treating the test material for this EUPT-FV-SM04 were mainly chosen taking

into account the following considerations:

that they were not included in the EU-Coordinated Multiannual Control Programme for

2011 (Regulation (EC) 915/2011).

that they had particularly acute toxicity and/or had low ARfD values.


Table 2.1 shows the 26 pesticides used to spike the pear sample.

Table 2.1. The spiked pesticides used.

Spiked Pesticides

Bromacil Fenpropidin Napropamide

Bromoxinyl Flufenacet Prometryn

Cadusafos Flutolanil Propaquizafop

Diflubenzuron Imazapyr Pyrifenox

Diniconazole Ioxynil Terbacil

Ethoxiquin Isoproturon Terbumeton

Etrimfos Metazachlor Vamidothion

2.2 Analytical methods

The two analytical methods described briefly below were used by the Organiser for the

homogeneity and stability tests performed by the EURL-FV. These were:

- GC method: The sample is extracted with ethyl acetate along with sodium chloride and

magnesium sulphate anhydrous. The mixture is shaken and centrifuged. The final extract

is injected into GC-MS/MS.

- LC method: The sample is extracted with ethyl acetate and sodium hydroxide. The

mixture is shaken and centrifuged. The extract is evaporated and redissolved in methanol

and directly injected into LC-MS/MS.

2.3 Prior analysis of the spiked pear test material

The Organiser’s homogeneity and stability tests associated with ‘quantitative’ PTs were

conducted with a further acceptance criterion to those in the classical EUPT-FVs - the PT test

material was analysed in order to detect the presence of the spiked pesticides, which were

consistently confirmed to be above the Organiser’s LOD.

To confirm the homogeneity of the test material sent, ten spiked test samples were randomly

chosen from those stored in the freezer and analysed in duplicate so as to check for the

presence of the pesticides.

The injection sequence of the 10 analyses by GC and LC was determined from a table of

randomly-generated numbers. The relative standard deviation (RSD) of these 20 analyses

needed to be at 15%, or below, to consider the material homogeneous.


Table 2.3.1 shows the results of these tests, together with the average concentration values for

each of the pesticides used to treat the sample along with the RSDs.

Table 2.3.1 Homogeneity tests

Test material No.

026 a

026 b

040a

040b

046a

046 b

054 a

054 b

074 a

074 b

078 a

078 b

081 a

081 b

114 a

114 b

132 a

132 b

141 a

141 b

A. Cc (µg/kg)

RSD (%)

Bromacil D D D D D D D D D D D D D D D D D D D D 437.7 8.4

Bromoxinyl D D D D D D D D D D D D D D D D D D D D 291.2 14.1

Cadusafos D D D D D D D D D D D D D D D D D D D D 209.4 10.6

Diflubenzuron D D D D D D D D D D D D D D D D D D D D 379.5 14.6

Diniconazole D D D D D D D D D D D D D D D D D D D D 209.2 8.2

Ethoxiquin D D D D D D D D D D D D D D D D D D D D 101.1 10.6

Etrimfos D D D D D D D D D D D D D D D D D D D D 56.5 1.1

Fenpropidin D D D D D D D D D D D D D D D D D D D D 59.5 12.5

Flufenacet D D D D D D D D D D D D D D D D D D D D 77.8 2.4

Flutolanil D D D D D D D D D D D D D D D D D D D D 79.8 2.3

Imazapyr D D D D D D D D D D D D D D D D D D D D 196.0 9.9

Ioxynil D D D D D D D D D D D D D D D D D D D D 148.1 10.6

Isoproturon D D D D D D D D D D D D D D D D D D D D 160.8 4.8

Metazachlor D D D D D D D D D D D D D D D D D D D D 80.2 2.7

Napropamide D D D D D D D D D D D D D D D D D D D D 51.6 1.5

Prometryn D D D D D D D D D D D D D D D D D D D D 62.7 1.6

Propaquizafop D D D D D D D D D D D D D D D D D D D D 16.5 4.5

Pyrifenox D D D D D D D D D D D D D D D D D D D D 37.5 4.2

Terbacil D D D D D D D D D D D D D D D D D D D D 204.6 8.3

Terbumeton D D D D D D D D D D D D D D D D D D D D 382.3 7.0

Vamidothion D D D D D D D D D D D D D D D D D D D D 95.4 10.9

D: Detected A. Cc: Average Concentration RSD: Relative Standard Deviation

Further analyses to test for stability were performed following varying time lapses. On each

occasion, a test material sample stored in the freezer at -20°C was randomly chosen and

analysed.

The three occasions were:

- Day 1: one week before the sample shipment on 10th February 2012.

- Day 2: on 20th February 2012 after reproducing the sample shipment conditions.

- Day 3: soon after the deadline for reporting results on 23rd February 2012.

For all the analyses, the two analytical methods described briefly above (in section 2.2) were

used.

All the pesticides used to spike the samples demonstrated sufficient stability even after

reproducing the 48h delivery conditions. All were detected on each occasion.


Table 2.3.2 Stability tests performed.

Stability tests Test material Number

057 Day 1

057 Day 1

062 Day 2

062 Day 2

137 Day 3

137 Day 3

Bromacil D D D D D D

Bromoxinyl D D D D D D

Cadusafos D D D D D D

Diflubenzuron D D D D D D

Diniconazole D D D D D D

Ethoxiquin D D D D D D

Etrimfos D D D D D D

Fenpropidin D D D D D D

Flufenacet D D D D D D

Flutolanil D D D D D D

Imazapyr D D D D D D

Ioxynil D D D D D D

Isoproturon D D D D D D

Metazachlor D D D D D D

Napropamide D D D D D D

Prometryn D D D D D D

Propaquizafop D D D D D D

Pyrifenox D D D D D D

Terbacil D D D D D D

Terbumeton D D D D D D

Vamidothion D D D D D D

D: Detected

2.4 Distribution of test materials and protocol to participants

Approximately 300 g of treated pear homogenate together with another 300 g of ‘blank’ pear

homogenate were shipped to participants on 20th February 2012. The deadline for results

submission to the Organiser was 72 hours after receipt of the test material. Participants were

asked to report all the pesticides that they detected.

Laboratories were asked to screen the test materials using the wide-scope screening methods

they would normally apply, or anticipate applying, for official monitoring purposes. This typically

involves full-scan techniques like GC-MS (full-scan quadrupole, ion trap, ToF) and/or LC-TOF-MS

and Orbitrap. However, extended targeted methods using LC tandem MS (triple quadrupole, Q-

trap, Q-TOF) or GC-MS/MS could also be used.

Before shipment, the laboratories received full instructions for the receipt and analysis of the

spiked test material although they were encouraged to use their own screening methods. These

instructions, laid out as the General and Specific Protocols, were uploaded onto the EUPT-FV-

SM04 web page, designed especially for this Proficiency Test. This information was also sent by e-

mail to all participant laboratories. The Application Form was uploaded onto this same web site

together with Form 0 (Sample Receipt) and Form 1 (Results). These allowed the evaluation of the

mass-spectrometric screening methods that each of the participants used.


3. STATISTICAL METHODS

3.1 Type of results reported

The results evaluation is concerned with the results themselves matching the pesticides that the

Organiser used to treat the sample; or otherwise stating a ‘not-reported pesticide’ or ‘other

reported pesticide’ from those used to treat the sample. After receiving the results, the Organiser

may consider further evaluation highlighted by important information received.

3.1.1 Other Reported Pesticides

These were considered as those results showing the apparent presence of pesticides which

were: (i) not used in the test material treatment, or (ii) not detected by the Organiser, even

after repeated analyses. However, if a number of participants detect the same additional

pesticide(s), then a decision as to whether, or not, this should be considered an ‘Other

Reported Pesticide’ result was made on a case-by-case basis.

Organiser’s Note:

Not all screening methods immediately provide sufficient information to

allow full identification. In such cases, when they detect a pesticide in

real life, laboratories normally do a follow-up confirmatory analysis:

using, for example, LC-MS/MS and based on two transitions. In future PTs

of this nature, there will be a need to distinguish between suspect or

tentative detection and full identification.

3.1.2 Not-Reported Pesticides

These were considered as any pesticides present in the sample but not reported by the lab

even though the Organiser had used it to spike the test material and it was detected by the

majority of participants.


4. RESULTS

4.1 Summary of reported results

Fifty-three laboratories agreed to participate in this fourth proficiency test on screening methods.

Fifty-one laboratories submitted results. All results reported by the participants are given in

Appendix 1. Graphical representations of the results reported are shown in Appendix 2. Details of

the screening methods used are provided in Appendix 3 (available only as a pdf document

uploaded to the EUPT-SM04 webpage, not in the printed version). The laboratories that agreed to

participate are listed in Annex 1.

A summary of the results reported by pesticide and by laboratory can be seen in Table 4.1.

Table 4.1 Summary of Results Reported.

Pesticide No. of Reported % of Reported* No. of Not Reported % of Not Reported*

Bromacil 44 86 7 14

Bromoxinyl 37 73 14 27

Cadusafos 46 90 5 10

Diflubenzuron 42 82 9 18

Diniconazole 47 92 4 8

Ethoxyquin 37 73 14 27

Etrimfos 48 94 3 6

Fenpropidin 44 86 7 14

Flufenacet 39 76 12 24

Flutolanil 43 84 8 16

Imazapyr 18 35 33 65

Ioxynil 28 55 23 45

Isoproturon 46 90 5 10

Metazachlor 45 88 6 12

Napropamide 43 84 8 16

Prometryn 45 88 6 12

Propaquizafop 24 47 27 53

Pyrifenox 40 78 11 22

Terbacil 38 75 13 25

Terbumeton 38 75 13 25

Vamidothion 36 71 15 29

Spinosad** 43 84 8 16

* The % of laboratories is calculated based on the total number of laboratories submitting results (51). ** Reported but not spiked


4.1.1 Other Reported Pesticides

Many laboratories reported additional pesticides to those used to spike the test material. These

reported pesticides are presented in Table 4.1.1.

Table 4.1.1. ‘Other reported pesticides’ in the test material given by laboratories.

LABORATORY CODE OTHER REPORTED PESTICIDES

Lab003* Secbumeton

Lab008 Atrazine-2-hydroxy, Atrazine-desethyl-2-hydroxy

Lab009* Ametryn, Carbaryl, Endosulfan alpha, Imibenconazol, Propiconazole, Terbutylazin

Lab010* 3-Chloroaniline, Prometon, Terbutryn, Secbumeton

Lab012* 3-Chloroaniline

Lab016 Formothion, Omethoate, Secbumeton

Lab017* Phenothrin, Photodieldrin, Tebufenocide, Thiodemeton

Lab019* 3-Chloroaniline

Lab020 3-Chloroaniline

Lab022 Terbutryn

Lab025 Cyproconazole, Diclobutrazol, Propiconazole

Lab028* Atrazine-desethyl-2-hydroxy

Lab029 Cymoxanil, Terbutryn

Lab030* Ametryn, Cyazofomid, Diclobutrazol, Molinate, Terbutryn

Lab040* 3-Chloroaniline, Atraton, Demeton O, Isobornyl Thiocyanoacetate

Lab044 Difenoconazole, Folpet, Procloraz

Lab045 Chlorbufam, o-Phenylphenol, Trichlorfon

Lab048 Atraton

Lab050 Bifenox

* National Reference Laboratories for Fruit and Vegetables from the EU participating in this test.

Those pesticides reported by more than two laboratories were analysed by the Organiser, but

none of these pesticides was detected after repeated analyses.

4.1.2 Not-Reported Pesticides

In Table 4.1, the number and percentage of laboratories not reporting each of the pesticides

used to spike the sample can be seen. The individual results for each laboratory are given in

Appendix 1. Graphical representations can be seen in Appendix 2.

4.2 Concentration levels.

Twenty-one pesticides were used to spike the pear test material at different levels, in the range

between 50 and 1000 µg/kg. Spinosad was present in the sample at around 5µg/kg. This EUPT was

focused only on detection capabilities; therefore no quantitative data were requested.


4.3 Assessment of laboratory performance.

No z-score values were carried out for laboratories to assess their performance as no numerical

results were reported by the participants. However, classification was considered important,

based on the number of detected results each laboratory reported and also on which methods

they used.

Table 4.3.1 classifies the laboratories according to the number of spiked pesticides reported.

Table 4.3.1 Classification of laboratories according to the number of spiked pesticides reported.

Laboratory Code Reported

Other Reported Pesticides

Not Confirmed by the Organiser

Confirmed by the Organiser

Lab024 22 0

Lab034* 22 0 Lab028* 22 1 Lab048 22 1 Lab008 22 2 0

Lab040* 22 4 0 Lab001 21 0 Lab014 21 0 Lab023 21 0

Lab049 21 0 0 Lab010* 21 4 0 Lab004* 20 0 Lab015 20 0

Lab038 20 0 Lab047* 20 0 Lab003* 20 1 Lab025 20 3 0

Lab006 19 0 Lab018 19 0 Lab021 19 0 Lab041 19 0

Lab046 19 0 Lab030* 19 5 Lab002* 18 0 Lab011 18 0

Lab031 18 0 0 Lab039 18 0 0 Lab043* 18 0 0 Lab020 18 1 0

Lab036 17 0 Lab037 17 0 Lab042 17 0 Lab019* 17 1 0

Lab016 17 3 0 Lab045 17 3 0 Lab026 16 0 Lab050 16 1


Laboratory Code Reported

Other Reported Pesticides

Not Confirmed by the Organiser

Confirmed by the Organiser

Lab029 16 2 0 Lab017* 16 4 0 Lab007* 15 0 Lab053 15 0

Lab009* 15 6 0 Lab027* 14 0

Lab012* 14 1 0

Lab033 13 0 0

Lab032 11 0

Lab051 11 0 0

Lab022 10 1

Lab035* 6 0

Lab013 1 0

Lab044 1 3 0

Lab005 No Results Reported

Lab052 No Results Reported * National Reference Laboratories for Fruit and Vegetables from the EU participating in this test.

The methods used by the laboratories, the chromatographic techniques, detectors,

instrumentation, etc… are detailed in Appendix 3 (available only as a pdf document uploaded

to the EUPT-SM04 webpage, not in the printed version). In Table 4.3.2, there is a summary of the

chromatographic techniques used for each pesticide, and a graphical representation is shown in

Appendix 2.

Table 4.3.2 Chromatographic techniques used to determine each pesticide in the test material

Pesticide Total no. of Reports GC Full-scan GC LC Full-scan LC

Bromacil 46 18 14 28 10

Bromoxinyl 39 11 11 28 6

Cadusafos 49 26 15 23 5

Diflubenzuron 44 3 2 41 10

Diniconazole 50 20 15 30 6

Ethoxyquin 39 24 17 15 4

Etrimfos 50 34 21 16 5

Fenpropidin 47 18 13 29 5

Flufenacet 41 14 12 27 7

Flutolanil 46 25 16 21 6

Imazapyr 18 0 0 18 4

Ioxynil 29 4 4 25 5

Isoproturon 46 2 2 44 10

Metazachlor 47 27 18 20 6


Pesticide Total no. of Reports GC Full-scan GC LC Full-scan LC

Napropamide 45 18 12 27 8

Prometryn 48 26 18 22 6

Propaquizafop 25 0 0 25 5

Pyrifenox 44 20 14 24 6

Spinosad* 53 0 0 53 13

Terbacil 39 30 20 9 6

Terbumeton 41 23 18 18 7

Vamidothion 44 5 5 39 7

*Spinosad was present in the sample but not spiked. Note: The number of reports for each of the pesticides could be different to the reports shown in Table 4.1 because a particular laboratory might analize each of the pesticides with more than one technique.

In Appendix 2, graphical representations of the techniques used can be seen.

Table 4.3.3 shows the number and percentage of the pesticides used by the Organiser to spike

the sample which were reported by each laboratory. National Reference Laboratories are

marked with an asterisk.

Table 4.3.3. Number and Percentage of Present Pesticides Reported by Laboratory

Laboratory Code

Number of Present Pesticides Reported

% of Present Pesticides Reported

Lab001 21 95

Lab002* 18 82

Lab003* 20 91

Lab004* 20 91

Lab006 19 86

Lab007* 15 68

Lab008 22 100

Lab009* 15 68

Lab010* 21 95

Lab011 18 82

Lab012* 14 64

Lab013 1 5

Lab014 21 95

Lab015 20 91

Lab016 17 77

Lab017* 16 73

Lab018 19 86

Lab019* 17 77

Lab020 18 82

Lab021 19 86

Lab022 10 45

Lab023 21 95


Laboratory Code

Number of Present Pesticides Reported

% of Present Pesticides Reported

Lab024 22 100

Lab025 20 91

Lab026 16 73

Lab027* 14 64

Lab028* 22 100

Lab029 16 73

Lab030* 19 86

Lab031 18 82

Lab032 11 50

Lab033 13 59

Lab034* 22 100

Lab035* 6 27

Lab036 17 77

Lab037 17 77

Lab038 20 91

Lab039 18 82

Lab040* 22 100

Lab041 19 86

Lab042 17 77

Lab043* 18 82

Lab044 1 5

Lab045 17 77

Lab046 19 86

Lab047* 20 91

Lab048 22 100

Lab049 21 95

Lab050 16 73

Lab051 11 50

Lab053 15 68

* National Reference Laboratories for Fruit and Vegetables from the EU participating in this test.


5. CONCLUSIONS

Fifty-three laboratories applied to participate in this test and fifty-one laboratories submitted

results. Seventeen of the laboratories which applied were National Reference Laboratories for

Fruit and Vegetables (marked with an asterisk on the graphs and tables) representing nineteen

Member States. In addition to these, 2 EFTA countries (Norway and Switzerland) and three non-

EU/EFTA countries (Egypt, Serbia and Turkey) participated in this European Union Proficiency Test.

Most laboratories analysed the test material using methods based on both gas and liquid

chromatography, combined with mass spectrometric detection. In the case of GC-MS analysis,

full-scan acquisition, with associated target-library software (covering a large number of

pesticides) was used by the majority of the laboratories. In the case of LC-MS analysis, targeted

acquisition methods using triple quadrupole instruments were the most widely used. Of 930

detections, 395 were made using full-scan, meaning 43% of detections; 248 by LC techniques

and 147 by GC techniques.

Four of the 53 laboratories were able to detect all 22 pesticides in the spiked pear test material

(21 spiked plus spinosad, which was present in the blank). Only 4 laboratories failed to detect less

than 50% of the pesticides present.

Seventy-six percent of the laboratories (39 laboratories) that reported results were able to find

more than 70% of the pesticides used to spike the sample whereas last year (EUPT-FV-SM03) only

71% managed to do so.

Nineteen participants reported thirty-two different pesticides which were not used for spiking the

pears. Whether this should be judged as poor performance, or not, depends on how each

participant would act on these positive findings in routine analysis. If the detected pesticide were

reported as positive with no further identifying confirmation, then the result would be a false

positive and hence erroneous monitoring data would be reported. If the detected pesticide is

regarded simply as ‘suspect’ or ‘indicatively present’, leading to additional analysis to confirm

identity before reporting the result, then those pesticides indicated as ‘other reported pesticides’

in this report are not really an issue.

This fourth interlaboratory test on wide-scope screening methods showed that such an approach

can substantially expand the scope of pesticide residue analysis. This is especially useful for

pesticides not frequently found in food and feed, or not monitored by the laboratories because

they are not part of the EU-Coordinated Programme. The use of screening methods can greatly

increase the chance of detecting less commonly found pesticides. However, the test also

revealed that improvements in scope (both in number and the choice of pesticides included)

and verification of the screening methods performance (i.e. validation) are necessary to improve

the reliability of such methods.


6. SUGGESTIONS FOR FUTURE WORK

The Organiser and the Scientific Committee consider that screening methods have provided

additional value to the current quantitative multiresidue methods routinely used for monitoring

purposes. The results of this fourth test are most encouraging, but also indicate the need for

continued evaluation of screening methods. Therefore, further proficiency tests will be organised

to provide support to those laboratories using screening methods in order to extend their use and

improve their reliability. These methods will be used more and more as screens/filters, to make

routine laboratory work easier and faster. The need for screening method validation has been

recognised and guidelines for such validation have been prepared and included in the updated

SANCO document: “Method validation and quality control procedures for pesticide residue

analysis in food and feed” (SANCO/12495/2011).

Next year, potato matrix test material will be used. If laboratories have a particular interest in

specific matrices, they should inform the EURL-FV and their suggestions will be evaluated. The

date of the test material delivery will be January 2013; and 72 hours will be allowed for results

submission (given that this should be enough time to carry out screening methods). There will be

no target list, as was the case in this test.


7. REFERENCES

Malato O., Lozano, A., Mezcua M., Agüera, A., and Fernandez-Alba A. R. Benefits and

pitfalls of the application of screening methods for the analysis of pesticide residues in

fruits and vegetables. Journal of Chromatography A, 2011, 1218(42), 7615-7626.

Mezcua M., Malato O., Martinez-Uroz M. A., Lozano, A., Agüera, A., and Fernandez-Alba

A. R. Evaluation of Relevant Time-of-Flight-MS Parameters Used in HPLC/MS Full-Scan

Screening Methods for Pesticides Residues. Journal of AOAC Int., 2011, 94 (6), 1674-1684.

Mezcua M., Martinez-Uroz M. A., Wylie P. L. and Fernandez-Alba A.R. Simultaneous

screening and target analytical approach by GC-q-MS for pesticide residues in fruits and

vegetables. Journal of AOAC Int., 2009, 92 (6).

Mezcua M., Malato O., Garcia-Reyes J. F., Molina-Diaz A., and Fernandez-Alba A. R.

Accurate-Mass Databases for Comprehensive Screening of Pesticide Residues in Food by

Fast Liquid Chromatography Time-of-Flight Mass Spectrometry. Anal. Chem. 2009, 81,

913–929.

Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food

and Feed, European Commission, Document No. SANCO/10684/2009.

ISO/IEC 17043:2010 Conformity assessment - General requirements for proficiency testing.


8. ACKNOWLEDGEMENTS

The Organiser is grateful to the European Commission for funding this 4th European Proficiency

Test for Screening Methods in Fruit and Vegetables.

The Organiser wishes to thank the members of the Scientific Committee for their invaluable and

knowledgeable advice.

The Organiser wishes to give a special thank-you to Almeria University for the use of their facilities.

APPENDIX 1. Results


Labo

rato

ry C

ode

Tota

l No

of

Repo

rting

La

bora

torie

s = 5

1 Evaluated Pesticides (21 added + 1 present in the blank)

Repo

rted

Pes

ticid

es

by L

abor

ator

y

% o

f Rep

orte

d Pe

stic

ides

by

Labo

rato

ry

Brom

acil

Brom

oxin

yl

Cad

usaf

os

Difl

uben

zuro

n

Din

icon

azol

e

Etho

xyqu

in

Etrim

fos

Fenp

ropi

din

Fluf

ena

cet

Flut

olan

il

Imaz

apyr

Ioxy

nil

Isopr

otur

on

Met

aza

chlo

r

Nap

ropa

mid

e

Prom

etry

n

Prop

aqui

zafo

p

Pyrif

enox

Terb

acil

Terb

umet

on

Vam

idot

hion

Spin

osad

001 R R R R R R R R R R R R R R R R R R R R R 21 95 002* R R R R R R R R R R R R R R R R R R 18 82 003* R R R R R R R R R R R R R R R R R R R R 20 91 004* R R R R R R R R R R R R R R R R R R R R 20 91 005 No Results Reported 0 0 006 R R R R R R R R R R R R R R R R R R R 19 86 007* R R R R R R R R R R R R R R R 15 68 008 R R R R R R R R R R R R R R R R R R R R R R 22 100 009* R R R R R R R R R R R R R R R 15 68 010* R R R R R R R R R R R R R R R R R R R R R 21 95 011 R R R R R R R R R R R R R R R R R R 18 82 012* R R R R R R R R R R R R R R 14 64 013 R 1 5 014 R R R R R R R R R R R R R R R R R R R R R 21 95 015 R R R R R R R R R R R R R R R R R R R R 20 91 016 R R R R R R R R R R R R R R R R R 17 77 017* R R R R R R R R R R R R R R R R 16 73 018 R R R R R R R R R R R R R R R R R R R 19 86 019* R R R R R R R R R R R R R R R R R 17 77 020 R R R R R R R R R R R R R R R R R R 18 82 021 R R R R R R R R R R R R R R R R R R R 19 86 022 R R R R R R R R R R 10 45 023 R R R R R R R R R R R R R R R R R R R R R 21 95 024 R R R R R R R R R R R R R R R R R R R R R R 22 100 025 R R R R R R R R R R R R R R R R R R R R 20 91 026 R R R R R R R R R R R R R R R R 16 73 027* R R R R R R R R R R R R R R 14 64 028* R R R R R R R R R R R R R R R R R R R R R R 22 100 029 R R R R R R R R R R R R R R R R 16 73 030* R R R R R R R R R R R R R R R R R R R 19 86 031 R R R R R R R R R R R R R R R R R R 18 82 032 R R R R R R R R R R R 11 50 033 R R R R R R R R R R R R R 13 59 034* R R R R R R R R R R R R R R R R R R R R R R 22 100 035* R R R R R R 6 27 036 R R R R R R R R R R R R R R R R R 17 77 037 R R R R R R R R R R R R R R R R R 17 77 038 R R R R R R R R R R R R R R R R R R R R 20 91 039 R R R R R R R R R R R R R R R R R R 18 82 040* R R R R R R R R R R R R R R R R R R R R R R 22 100 041 R R R R R R R R R R R R R R R R R R R 19 86 042 R R R R R R R R R R R R R R R R R 17 77 043* R R R R R R R R R R R R R R R R R R 18 82 044 R 1 5 045 R R R R R R R R R R R R R R R R R 17 77 046 R R R R R R R R R R R R R R R R R R R 19 86 047* R R R R R R R R R R R R R R R R R R R R 20 91 048 R R R R R R R R R R R R R R R R R R R R R R 22 100 049 R R R R R R R R R R R R R R R R R R R R R 21 95 050 R R R R R R R R R R R R R R R R 16 73 051 R R R R R R R R R R R 11 50 052 No Results Reported 0 0 053 R R R R R R R R R R R R R R R 15 68

Reported Pesticides 44 37 46 42 47 37 48 44 39 43 18 28 46 45 43 45 24 40 38 38 36 43

% of Reported

Pesticides 86 73 90 82 92 73 94 86 76 84 35 55 90 88 84 88 47 78 75 75 71 84

R: Reported pesticide * NRLs from EU

APPENDIX 2. Graphical Representations


1 16

10 1

11

11

3 14

14 1

51

51

5 16

16

16

16 1

71

71

71

71

71

7 18

18

18

18

18

18 1

91

91

91

91

91

9 20

20

20

20

20

20 2

12

12

12

12

1 22

22

22

22

22

22

0

2

4

6

8

10

12

14

16

18

20

22

24

Lab0

13

Lab0

44

Lab0

35

*Lab

02

2Lab

03

2Lab

05

1Lab

03

3Lab

01

2*

Lab0

27

*Lab

00

7*

Lab0

09

*Lab

05

3Lab

01

7*

Lab0

26

Lab0

29

Lab0

50

Lab0

16

Lab0

19

*Lab

03

6Lab

03

7Lab

04

2Lab

04

5Lab

00

2*

Lab0

11

Lab0

20

Lab0

31

Lab0

39

Lab0

43

*Lab

00

6Lab

01

8Lab

02

1Lab

03

0*

Lab0

41

Lab0

46

Lab0

03

*Lab

00

4*

Lab0

15

Lab0

25

Lab0

38

Lab0

47

*Lab

00

1Lab

01

0*

Lab0

14

Lab0

23

Lab0

49

Lab0

08

Lab0

24

Lab0

28

*Lab

03

4*

Lab0

40

*Lab

04

8N

o o

f R

ep

ort

ed

Pe

stic

ide

s

Number of Reported Data by Laboratory(*NRL) (22 Pesticides Included)

5 52

74

5 50

50

59 6

46

4 68

68

68 7

37

37

37

3 77

77

77

77

77

77 8

28

28

28

28

28

2 86

86

86

86

86

86 9

19

19

19

19

19

1 95

95

95

95

95 1

00

10

01

00

10

01

00

10

0

0

10

20

30

40

50

60

70

80

90

100

Lab0

13

Lab0

44

Lab0

35

*Lab

02

2Lab

03

2Lab

05

1Lab

03

3Lab

01

2*

Lab0

27

*Lab

00

7*

Lab0

09

*Lab

05

3Lab

01

7*

Lab0

26

Lab0

29

Lab0

50

Lab0

16

Lab0

19

*Lab

03

6Lab

03

7Lab

04

2Lab

04

5Lab

00

2*

Lab0

11

Lab0

20

Lab0

31

Lab0

39

Lab0

43

*Lab

00

6Lab

01

8Lab

02

1Lab

03

0*

Lab0

41

Lab0

46

Lab0

03

*Lab

00

4*

Lab0

15

Lab0

25

Lab0

38

Lab0

47

*Lab

00

1Lab

01

0*

Lab0

14

Lab0

23

Lab0

49

Lab0

08

Lab0

24

Lab0

28

*Lab

03

4*

Lab0

40

*Lab

04

8%

of

Re

po

rte

d P

est

icid

es

% of Reported Data by Laboratory(*NRL) (22 Pesticides Included)



0 0 0 0 0 01 1 1 1 1

2 2 2 2 2 23 3 3 3 3 3

4 4 4 4 4 45 5 5 5 5 5

6 6 6 67 7 7

8 89

11

11 1

21

62

12

1

0

2

4

6

8

10

12

14

16

18

20

22

24

26

Lab0

08

Lab0

24

Lab0

28

*Lab

03

4*

Lab0

40

*Lab

04

8Lab

00

1Lab

01

0*

Lab0

14

Lab0

23

Lab0

49

Lab0

03

*Lab

00

4*

Lab0

15

Lab0

25

Lab0

38

Lab0

47

*Lab

00

6Lab

01

8Lab

02

1Lab

03

0*

Lab0

41

Lab0

46

Lab0

02

*Lab

01

1Lab

02

0Lab

03

1Lab

03

9Lab

04

3*

Lab0

16

Lab0

19

*Lab

03

6Lab

03

7Lab

04

2Lab

04

5Lab

01

7*

Lab0

26

Lab0

29

Lab0

50

Lab0

07

*Lab

00

9*

Lab0

53

Lab0

12

*Lab

02

7*

Lab0

33

Lab0

32

Lab0

51

Lab0

22

Lab0

35

*Lab

01

3Lab

04

4N

o o

f N

ot

Re

po

rte

d P

est

icid

es

SM04 Not Reported Pesticides(*NRL)

0 0 0 0 0 05 5 5 5 5

9 9 9 9 9 91

41

41

41

41

41

4 18

18

18

18

18

18 2

32

32

32

32

32

3 27

27

27

27 3

23

23

2 36

36 4

15

05

0 55

73

95

95

0

10

20

30

40

50

60

70

80

90

100

Lab0

08

Lab0

24

Lab0

28

*Lab

03

4*

Lab0

40

*Lab

04

8Lab

00

1Lab

01

0*

Lab0

14

Lab0

23

Lab0

49

Lab0

03

*Lab

00

4*

Lab0

15

Lab0

25

Lab0

38

Lab0

47

*Lab

00

6Lab

01

8Lab

02

1Lab

03

0*

Lab0

41

Lab0

46

Lab0

02

*Lab

01

1Lab

02

0Lab

03

1Lab

03

9Lab

04

3*

Lab0

16

Lab0

19

*Lab

03

6Lab

03

7Lab

04

2Lab

04

5Lab

01

7*

Lab0

26

Lab0

29

Lab0

50

Lab0

07

*Lab

00

9*

Lab0

53

Lab0

12

*Lab

02

7*

Lab0

33

Lab0

32

Lab0

51

Lab0

22

Lab0

35

*Lab

01

3Lab

04

4%

of

No

t R

ep

ort

ed

Pe

stic

ide

s

SM04 % of Not Reported Pesticides(*NRL)



44

37

46

42

47

37

48

44

39

43

18

28

46

45

43

45

24

40

43

38

38

36

0

10

20

30

40

50

60

Bro

macil

Bro

mo

xinyl

Cad

usafo

s

Diflu

be

nzu

ron

Din

icon

azole

Etho

xyqu

in

Etrimfo

s

Fen

pro

pid

in

Flufe

nace

t

Fluto

lanil

Imazap

yr

Ioxyn

il

Isop

rotu

ron

Metazach

lor

Nap

rop

amid

e

Pro

metryn

Pro

paq

uizafo

p

Pyrifen

ox

Spin

osad

Terb

acil

Terb

um

eton

Vam

ido

thio

nN

o o

f D

ete

ctio

ns

SM04 Number of Reported Data by Pesticide(51 Laboratories Reported Data)

86 73 90 82 92 73 94 86 76 84 35 55 90 88 84 88 47 78 84 75 75 71

0

10

20

30

40

50

60

70

80

90

100

Bro

macil

Bro

mo

xinyl

Cad

usafo

s

Diflu

ben

zuro

n

Din

icon

azole

Etho

xyqu

in

Etrimfo

s

Fenp

rop

idin

Flufe

nace

t

Fluto

lanil

Imazap

yr

Ioxyn

il

Isop

rotu

ron

Metazach

lor

Nap

rop

amid

e

Pro

metryn

Pro

paq

uizafo

p

Pyrifen

ox

Spin

osad

Terb

acil

Terb

um

eto

n

Vam

ido

thio

n%

of

Det

ect

ion

s

SM04 % of Reported Data by Pesticide(51 Laboratories Reported Data)



Chromatographic Techniques used in Full Scan to determine each pesticide in the test material

46

39

49

44

50

39

50

47

41

46

18

29

46 47 45

48

25

44

53

39 41

44

14

11

15

2

15 17

21

13 12

16

0

4 2

18

12

18

0

14

0

20 18

5

10

6 5

10

6 4 5 5 7 6 4 5

10

6 8 6 5 6

13

6 7 7

0

10

20

30

40

50

60

Broma

cil

Bromoxinyl

Cadusafos

Diflubenzuron

Dinicona

zole

Ethoxyquin

Etrimfos

Fenprop

idin

Flufenacet

Flutolanil

Imaza

pyr

Ioxynil

Isoproturon

Metazachlor

Nap

ropam

ide

Prometryn

Propaquizafop

Pyrifenox

Spinosad

Terbacil

Terbum

eton

Va

midothion

No

of R

epor

ted

Dete

ctio

ns

SM4 Techniques (Full Scan)

Total Reported Full Scan GC Full Scan LC

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

23

BR

OM

AC

IL

Laboratory Code

How was the identification done?

RT Deviation (in seconds)

MS Tolerance (ppm)

Other Identification Details

Chromatographic Techique

Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?

Screening Reporting Level (SRL) Range?

Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type

Injecton Volume (µL)

Software

Compounds in method or library

(pesticides ONLY)

Standard Solution Frequency

001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

11.2

G

C

MSD

Q

EI

+

YES

YES

not

valid

ated

YE

S A

T 59

75

10

AC

N

SPE

HP5-

MS

10

Aut

o ap

rox

750

Alw

ays

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S N

O

NA

N

O

Agi

lent

646

0,

1290

HPLC

10

Et

OA

c N

one

Wa

ters

, HSS

T3,

15

0 x

2.1m

m

2 Bo

th

500

Each

Ba

tch

004

Con

firm

ed w

ith

seco

nd m

etho

d

-1.8

0.

6

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch

Batc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

6.3

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch

Batc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.01

0 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

24

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

BR

OM

AC

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT ES

I -

YES

YES

0.01

N

O

10

A

CN

Both

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.01

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.1

2 1.

2 iso

tope

, 2 io

ns

< 5p

pm

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

86

0 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

028

Con

firm

ed w

ith

seco

nd m

etho

d

261.

0>20

5.0,

26

1.0>

187.

0 LC

M

SD

QQ

Q

ESI

+ N

O

NO

10-

100

ppb

N

O

LC: A

gile

nt 1

200,

M

S:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o 59

1

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch

Batc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

25

BR

OM

AC

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

025-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

pel

quad

ropo

l, Sc

iex

10

EtO

Ac

Filte

r HS

S T3

2

Both

14

1 Ea

ch

Batc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-5.5

20

%

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01

YES

Agi

lent

GC

-MSD

78

90A

/597

5c

10

AC

N

PSA

, C18

HP

-5M

S 1

Aut

o 92

7

034

Con

firm

ed w

ith

seco

nd m

etho

d

full

scan

G

C

MSD

Q

EI

+

NO

N

O

YE

S A

gile

nt 5

973

MSD

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 10

Bo

th

950

035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

040

Con

firm

ed w

ith

seco

nd m

etho

d

3 1

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

20

%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch

Batc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch

Batc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

26

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

BR

OM

AC

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.8

Spec

trum

m

atch

(re

vers

ed)

GC

M

SD

IT EI

+

YES

YES

20-1

0.00

0 µg

/kg

YES

Var

ian

Satu

rn

2000

15

A

ceto

ne/P

E/D

CM

N

O

VF-

5-m

s 5

Both

55

0 Q

uarte

rly

048

Con

firm

ed w

ith

seco

nd m

etho

d

8

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

18

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

120

0 LC

+646

0QQ

Q

10

AC

N

DSP

E YM

C T

riart

C18

2*

100

mm

3µm

5

Both

35

4 D

aily

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

8

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

27

BR

OM

OX

INY

L

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2

tran

sitio

ns

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

Agi

lent

649

0 5

ACN

RP-

C18

10

Bot

h

Dai

ly

002

Con

firm

ed w

ith

seco

nd m

etho

d 9.

8

G

C

MSD

Q

EI

+

YE

S

YES

not

valid

ated

YE

S

AT

5975

10

ACN

SPE

H

P5-M

S

10

Aut

o ap

rox

750

Alw

ays

003

Con

firm

ed w

ith

seco

nd m

etho

d 0.

05

5 2

tran

sitio

ns

LC

Q

-TO

F ES

I +

N

O

NO

YES

Bru

ker

Max

is

10

ACN

PS

A

RSLC

C18

1

Bot

h ap

rox

400

004

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

N

A

NA

LC

M

SD

Q

QQ

ES

I -

YES

NO

N

A

NO

Agi

lent

646

0,

1290

HPL

C

10

EtO

Ac

Non

e W

ater

s, H

SS T

3,

150

x 2.

1mm

2

Bot

h 50

0 Ea

ch B

atch

006

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

<

2 0

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES

>0.

010

mg/

kg

NO

W

ater

s qu

attr

o pr

emie

r 15

ACN

N

one

BEH

C18

10

Bot

h

008

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

1

2

tran

sitio

ns

+ac

cura

te

mas

s LC

M

SD

Q

-TRAP

ESI

- YE

S

NO

0.

01

NO

Q

Trap

550

0 10

ACN

N

one

reve

rsed

pha

se

3 Aut

o 30

0 Ea

ch B

atch

009

Tent

ativ

e de

tect

ed

2 tr

ansi

tions

LC

QQ

Q

ESI

- N

O

NO

NO

API

4000

10

ACN

D

SPE

Syn

ergi

e Fu

sion

RP8

0A

8 M

anua

l 40

Sch

edul

ed

MRM

M

etho

d al

so u

sed

for

quan

tific

atio

n

010

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2

tran

sitio

ns

LC

MSD

Q

QQ

ES

I +

N

O

YES

0.01

N

O

ABI4

000

10

ACN

N

O

C18

55

Bot

h ap

rox

580

Alw

ays

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

0.

2

2 tr

ansi

tions

G

C

MSD

Q

EI

+

YE

S

YES

0.01

YE

S

HP5

975C

10

ACN

D

SPE

H

P5M

S

10

Bot

h ap

rox

1000

Alw

ays

011

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

N

A

NA

NA

GC

MSD

Q

EI

+

N

O

NO

N

A

YES

5790

msd

10

ACN

PS

A

HP-

5MS

20

Aut

o 60

0 ap

rox

0-1

014

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

±

2.5%

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.01

0 m

g/kg

YE

S

Wat

ers-

TQD

15

ACN

PS

A

UPL

C-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atch

015

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

N

A

NA

2 tr

ansi

tions

LC

QQ

Q

ESI

+

YES

YES

0.01

N

O

6460

10

ACN

PS

A

C18

-XB

2 Bot

h 44

0

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

28

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

BR

OM

OX

INY

L

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


017

Tent

ativ

e de

tect

ed

G

C

MSD

TO

F EI

NO

N

O

YE

S

LECO

PEG

ASU

S

15

Ace

tone

/PE/

DCM

N

O

DB-5

1

Bot

h

018

Tent

ativ

e de

tect

ed

RT

lock

ing

2

tran

sitio

ns

GC

MSD

Q

EI

+

YE

S

YES

0.01

-0.0

5 m

g/kg

YE

S

Agi

lent

MSD

59

75B

10

ACN

PS

A

HP5

10

Bot

h >

600

Alw

ays

019

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

3

2

tran

sitio

ns

LC

MSD

Q

QQ

ES

I -

YES

YES

10

NO

Agi

lent

649

0 15

ACN

PS

A

C18

5

Aut

o

021

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

15

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.01

N

O

HPL

C A

gile

nt

1100

, M

S A

PI

3000

10

ACN

D

SPE

(PS

A,

MgS

O4)

C18

3µ

50x2

mm

10

Bot

h 55

0 Alw

ays

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT

ES

I -

YES

YES

0.01

N

O

10

ACN

Bot

h

Each

Bat

ch

024

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

0.

1

2 x

MRM

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.01

N

O

AB S

ciex

API

40

00

10

ACN

PS

A

Phen

omen

ex C

18

10

Bot

h 50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d 0.

04

1.0

isot

ope

LC

MSD

O

rbitr

ap

ESI

- N

O

NO

0.

01-0

.1

YES

Exac

tive

10

ACN

N

one

C18

Atla

ntis

T3

5 Bot

h 57

0 Ea

ch B

atch

Con

firm

ed w

ith

seco

nd m

etho

d N

A

776

spec

trum

G

C

MSD

TO

F EI

+

YE

S

YES

0.01

-0.1

YE

S L

eco

Pega

sus

IV 1

0 ACN

D

SPE

(PS

A)

RTX

-CL

pest

10

Aut

o 55

7 Ea

ch B

atch

026

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

<

0.5%

2.

5

GC

MSD

io

n tr

ap

EI

YE

S

YES

0.01

YE

S

Trap

400

0 -

Var

ian

10

ACN

D

SPE

5%

1

µL

Aut

o 45

0 Ev

ery

Wee

k

028

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

27

3.7>

78.9

, 27

5.4>

81.0

LC

M

SD

Q

QQ

ES

I -

YES

YES L

OQ

:2 p

pb

NO

LC

: Agi

lent

12

00,

MS:

API

40

00 Q

TRAP

10

ACN

Q

uEChE

RS

with

out

PSA

Sup

elco

Dis

cove

ry

C18

, 15

0 m

m x

2.

1 m

m,

5 µm

2

Aut

o

030

Tent

ativ

e de

tect

ed

LC

QQ

Q

ESI

+

YES

YES

0.02

N

O

Var

ian

320

15

ACN

C18

10

Aut

o 15

0 Ea

ch B

atch

031

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2

tran

sitio

ns

LC

MS/M

S

QQ

Q

ESI

- YE

S

YES

0.00

5-0.

04

µg/m

l N

O

UPL

C-M

SM

S

(Wat

ers

Aqu

ity

UPL

C s

yste

m,

API

500

0 Tr

ipel

quad

ropo

l, Sci

ex

5 Et

OAc

Filte

r H

SS T

3 2

Bot

h 25

0 Ea

ch B

atch

032

Tent

ativ

e de

tect

ed

0

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.01

N

O

Wat

ers

Acq

uity

TQ

D

10

Met

hano

l Fi

lter

C18

6

Aut

o 15

0 Alw

ays

034

Con

firm

ed w

ith

seco

nd m

etho

d

fu

ll sc

an

GC

MSD

Q

EI

+

N

O

NO

YES

Agi

lent

597

3 M

SD

10

ACN

D

SPE

(P

SA/M

gSO

4)

HP-

5MS

10

Bot

h 95

0

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

29

BR

OM

OX

INY

L

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


037

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2

tran

sitio

ns

LC

MS/M

S

QQ

Q

ESI

- YE

S

YES

0.01

0 N

O

4000

QTR

AP

10

ACN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

Alw

ays

038

Tent

ativ

e de

tect

ed

Non

e N

one

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

NO

N

O

N

O

API

400

0 10

ACN

D

SPE

W

ater

s-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Tent

ativ

e de

tect

ed

G

C

MSD

Q

EI

+

N

O

NO

YES

HP5

973

MSD

10

ACN

D

SPE

H

P-5M

SI

20

Bot

h 62

4 N

o st

anda

rd

used

040

Con

firm

ed w

ith

seco

nd m

etho

d 10

3

LC

TOF

ESI

- N

O

NO

YES

Agi

lent

623

0 10

ACN

N

one

Eclip

se C

18

3 Aut

o ap

rox

500

041

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2.

5%

2

tran

sitio

ns

LC

MSD

Q

QQ

ES

I -

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

ACN

PS

A

ZO

RBAX-E

CLI

PSE

XD

B-C

8 80

Aut

o 14

3

042

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2

tran

sitio

ns

LC

MSD

Q

QQ

ES

I -

YES

YES

N

O

API

400

0 10

ACN

Q

uEChE

RS

C18

Aqu

a 10

Bot

h

043

Tent

ativ

e de

tect

ed

0 0

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.01

0 YE

S

Api

320

0QT

10

ACN

D

SPE

Ph

enom

enex

fus

ion

10

Aut

o 20

0 D

aily

045

Tent

ativ

e de

tect

ed

1 1

unit

G

C

MSD

Q

EI

YES

NO

0.

01 p

pm

YES

Agi

lent

597

3 10

ACN

PS

A

HP

5 M

S U

I 2

Aut

o 92

3 Ea

ch B

atch

047

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

2.

4

2 tr

ansi

tions

+

ion

ratio

LC

M

SD

Q

QQ

ES

I -

NO

N

O

5-10

00

µg/k

g N

O

Wat

ers

Qua

ttro

Pr

emie

r XE

15

Ace

tone

/PE/

DCM

N

O

Allt

ima

C18

(1

50x3

mm

i.d.

) 5

Bot

h 27

Ea

ch B

atch

048

Con

firm

ed w

ith

seco

nd m

etho

d 0.

9

LC

M

SD

Q

QQ

ES

I -

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

ACN

D

SPE

(PSA)

Luna

C18

5

Bot

h 35

0 D

aily

049

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

0

2

tran

sitio

ns

LC

Q

QQ

ES

I +

YE

S

YES

N

O

Wat

ers

XEV

O

TQ M

S

10

ACN

BEH

C18

1,7

µm

3 Bot

h 60

D

aily

050

Fully

iden

tifie

d (S

AN

CO

/124

95/2

011

p.74

-80)

-0

.016

2 tr

ansi

tions

LC

M

SD

Q

QQ

ES

I -

YES

YES 0

.01-

0.05

YE

S

Agi

lent

120

0 LC

+64

60Q

QQ

10

ACN

D

SPE

YM

C T

riar

t C18

2*

100

mm

3µm

5

Bot

h 7

Dai

ly

051

Tent

ativ

e de

tect

ed

0.

5 qu

alifi

ers

GC

MSD

IT

EI

NO

N

O

YE

S

varian

GCM

S

4000

10

ACN

PS

A

varian

fac

tor

four

5

Bot

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

30

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

CA

DU

SA

FOS

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

6.8

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Ther

mo

TSQ

Q

uant

um X

LS

10

EtO

Ac

Non

e Th

erm

o TG

-5SI

LMS,

30

m*0

.25m

m*

0.25

um

2 A

uto

500

Each

Ba

tch

Con

firm

ed w

ith

seco

nd m

etho

d

1.2

0.4

LC

M

SD

TOF

ESI

+ N

O

NO

N

A

YES

Bruk

er M

axis

10

EtO

Ac

Non

e A

ccla

im R

SLC

120

C

18, 2

,1*1

00 m

m

1 Bo

th

1000

Ea

ch B

atc

h

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

36

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

NO

N

O

N

O

API

4000

10

A

CN

D

SPE

Syne

rgie

Fus

ion

RP80

A

8 M

anua

l 25

0

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

5.0

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

31

CA

DU

SA

FOS

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

EI

+

NO

YE

S 0.

010

NO

G

C-M

S/M

S (A

gile

nt)

15

AC

N

QuE

ChE

RS

DB

5MS

1 Bo

th

130

Alw

ays

017

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

TO

F EI

YES

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl 5

%

phen

yl si

loxa

ne

2 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, MS

API

30

00

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.01

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

2 -0

.05

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

92

5 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

32

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

CA

DU

SA

FOS

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

4 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

G

C +

320

-MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

271.

1>21

5.0,

27

1.1>

159.

0 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S LO

Q: 2

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o

029

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

S/M

S Q

QQ

EI

+

YES

YES

0.00

5-0.

64

µg/m

l N

O

Wa

ters

Qua

ttro

Mic

ro G

C

10

EtO

Ac

Filte

r Rx

i-5sil

MS/

inte

gra-

guar

d R

este

k 10

Bo

th

373

Each

Ba

tch

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3.5

m

in 3

ions

G

C

MSD

Q

EI

+

YES

NO

0.

01

YES

Agi

lent

GC

-MSD

78

90A

/597

5c

10

AC

N

PSA

, C18

HP

-5M

S 1

Aut

o 92

7

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

+ YE

S

10

A

CN

5

Aut

o 24

0

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

271.

1->1

59.0

, 27

1.1-

>130

.9

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

641

0B

10

AC

N

DSP

E C

18

2 Bo

th

187

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 5

973

30

EtO

Ac

HPG

PC

DB-

5MS

2 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

33

CA

DU

SA

FOS

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

G

C

MSD

Q

QQ

EI

+

YES

YES

N

O

Ther

mo

TSQ

Q

uant

um G

C

10

Ace

tone

/PE/

DC

M

Na2

SO4

RXi-5

SIL

MS

1 Bo

th

199

Each

Ba

tch

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

Spec

trum

m

atch

(re

vers

ed)

GC

M

SD

IT EI

+

YES

YES

20-1

0.00

0 µg

/kg

YES

Var

ian

Satu

rn

2000

15

A

ceto

ne/P

E/D

CM

N

O

VF-

5-m

s 5

Both

55

0 Q

uarte

rly

048

Con

firm

ed w

ith

seco

nd m

etho

d

5

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.02

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

354

Dai

ly

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

34

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

DIF

LUB

ENZ

UR

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software

Compounds in method or library (pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Aut

o 50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

-2.4

0

LC

M

SD

TOF

ESI

+ N

O

NO

N

A

YES

Bruk

er M

axis

10

EtO

Ac

Non

e A

ccla

im R

SLC

120

C

18, 2

,1*1

00 m

m

1 Bo

th

1000

Ea

ch B

atc

h

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

01

NO

A

gile

nt 6

410

10

AC

N

DSP

E Ec

lipse

XD

B-C

18

4 M

anua

l 13

9 Ea

ch B

atc

h

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

35

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

(=RL

) N

O

API

4000

10

A

CN

D

SPE

Syne

rgie

Fus

ion

RP80

A

8 M

anua

l 25

0

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

ABI

4000

10

A

CN

N

O

C18

55

Bo

th

apro

x 58

0 A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

NO

32

00q

trap

10

A

CN

PS

A

T-3

5 M

anua

l 17

0 1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

35

DIF

LUB

ENZ

UR

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

TO

F EI

YES

YES

YE

S LE

CO

PEG

ASU

S 15

A

ceto

ne/P

E/D

CM

N

O

DB-

5 1

Both

018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E (P

SA, M

gSO

4)

C18

3µ

50x2

mm

10

Bo

th

550

Alw

ays

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT ES

I -

YES

YES

0.01

N

O

10

A

CN

Both

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.1

9 -1

.0

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

4 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar +

32

0-M

S 10

A

CN

D

SPE

with

PSA

Re

stek

Ultr

a C

18

10

Both

30

2 Ea

ch B

atc

h

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

311.

1>15

8.2,

31

1.1>

141.

2 LC

M

SD

QQ

Q

ESI

- YE

S YE

S LO

Q: 2

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

36

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

DIF

LUB

ENZ

UR

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I -

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

- YE

S YE

S 0.

005-

0.4

µg/m

l N

O

Wa

ters

Aqu

ity

UPLC

syst

em,

API

500

0 Tr

ipel

quad

ropo

l, Sc

iex

10

EtO

Ac

Filte

r HS

S T3

2

Both

13

Ea

ch B

atc

h

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

- YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

311.

0->1

58.0

, 31

1.0-

>141

.0

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

641

0B

10

AC

N

DSP

E C

18

2 Bo

th

187

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

4 4

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T G

-64

10A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

80

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.4

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

- N

O

NO

5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

lltim

a C

18

(150

x3 m

m i.

d.)

5 Bo

th

27

Each

Ba

tch

048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

005

NO

A

gile

nt 6

410

10

AC

N

DSP

E(PS

A)

Luna

C18

5

Both

35

0 D

aily

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

37

DIF

LUB

ENZ

UR

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.01

9

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

354

Dai

ly

051

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.05

ABS

ciex

API

200

0 10

A

CN

PS

A

wat

ers A

tlant

is 5

Aut

o 11

7 Ea

ch B

atc

h

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

38

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

DIN

ICO

NA

ZO

LE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

5.3

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S N

O

NA

N

O

Agi

lent

646

0,

1290

HPLC

10

Et

OA

c N

one

Wa

ters

, HSS

T3,

150

x

2.1m

m

2 Bo

th

500

Each

Ba

tch

Con

firm

ed w

ith

seco

nd m

etho

d

-0.6

0.

3

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons+

accu

rate

mas

s LC

M

SD

Q-T

RAP

ESI

+ YE

S N

O

0.01

N

O

QTr

ap 5

500

10

AC

N

Non

e re

vers

ed p

hase

2.

5 A

uto

300

Each

Ba

tch

009

Con

firm

ed w

ith

seco

nd m

etho

d

21

2

trans

ition

s LC

QQ

Q

ESI

+ YE

S YE

S 0.

01 (=

RL)

NO

A

PI55

00

10

AC

N

DSP

E Sy

nerg

ie F

usio

n RP

80A

8

Man

ual

35

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

ABI

4000

10

A

CN

N

O

C18

55

Bo

th

apro

x 58

0 A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

0 N

O

Var

ian

320

50

Ace

tone

L/

L D

B5 ty

pe

8 Bo

th

146

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

39

DIN

ICO

NA

ZO

LE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E (P

SA, M

gSO

4)

C18

3µ

50x2

mm

10

Bo

th

550

Alw

ays

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

TO

F

YE

S YE

S 0.

01

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E Ph

enom

enen

x

ZB-5

MS

3 Bo

th

750

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

0.

03

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

92

3 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

Var

ian

10

AC

N

DSP

E 5%

1

µL

Aut

o 45

0 Ev

ery

Wee

k

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar

+320

-MS

10

AC

N

DSP

E w

ith P

SA

Rest

ek U

ltra

C18

10

Bo

th

302

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

40

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

DIN

ICO

NA

ZO

LE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

326.

1>70

.1,

328.

1>70

.1

LC

MSD

Q

QQ

ES

I +

YES

YES

LOQ

: 8

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

025-

0.25

µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

14

1 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Ther

mo

TSQ

Q

uant

um X

LS

Ultra

10

A

CN

PS

A

Cap

illary

1

Both

15

0 A

lway

s

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.9

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.01

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Tent

ativ

e d

etec

ted

5

4

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

41

DIN

ICO

NA

ZO

LE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons +

io

n ra

tio

LC

MSD

Q

QQ

ES

I +

YES

YES

5-10

00

µg/k

g N

O

Wa

ters

Qua

ttro

Prem

ier X

E 15

A

ceto

ne/P

E/D

CM

N

O

Acq

uity

BEH

(1

00x2

.1 m

m i.

d.)

5 Bo

th

230

Each

Ba

tch

048

Con

firm

ed w

ith

seco

nd m

etho

d

6

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

26

Q

ion

ratio

G

C

MSD

Q

EI

+

YES

YES

0.01

-0.0

5 YE

S A

gile

nt

6890

GC

+597

5MS

10

AC

N

DSP

E RE

STEK

-5M

S 50

Bo

th

168

Dai

ly

051

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

0.5

qual

ifier

s G

C

MSD

IT

EI

YE

S YE

S 0.

01

YES

Var

ian

GC

MS

4000

10

A

CN

PS

A

varia

n fa

ctor

four

5

Both

13

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

120

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

05

A

BSci

ex A

PI 2

000

10

AC

N

PSA

w

ater

s Atla

ntis

5 A

uto

117

Each

Ba

tch

053

Tent

ativ

e d

etec

ted

8

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

42

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ETH

OX

IQU

IN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

3.0

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

-1.2

1.

9

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S N

O

NA

N

O

Agi

lent

646

0,

1290

HPLC

10

Et

OA

c N

one

Wa

ters

, HSS

T3,

15

0 x

2.1m

m

2 Bo

th

500

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

10

Both

008

Tent

ativ

e d

etec

ted

2

trans

ition

s LC

M

SD

Q-T

RAP

ESI

+ N

O

NO

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 W

e d

o no

t ha

ve a

st

and

ard

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 80

Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.3

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±0.5

%

GC

M

SD

Q

EI

+ YE

S YE

S 0.

010

mg/

kg

YES

Agi

lent

789

0-59

75C

15

A

CN

PS

A

HP-5

MS

10

Aut

o 21

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

43

ETH

OX

IQU

IN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, MS

API

30

00

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d

NA

<

5 iso

tope

, 2 io

ns

< 5p

pm

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Con

firm

ed w

ith

seco

nd m

etho

d

< 20

85

4 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Mat

ch w

ith

anal

ytic

al

stan

dar

d

(Ma

tch

819,

ra

nge

0-10

00)

GC

M

SD

TOF

EI

YE

S YE

S LO

Q: 1

0 pp

b

YES

GC

xGC

-TO

F M

S Pe

gasu

s 4D

10

A

CN

Q

uEC

hERS

w

ithou

t PSA

DB5

-MS

(30

m x

0,2

5 m

m x

0,2

5 µm

) in

the

1st D

imen

sion,

BP

X-50

(2 m

x 0

,1

mm

x 0

,1 µ

m) i

n th

e 2n

d D

imen

sion

10

Aut

o

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

S/M

S Q

QQ

EI

+

YES

YES

0.02

5-0.

25

µg/m

l N

O

Wa

ters

Qua

ttro

Mic

ro G

C

10

EtO

Ac

Filte

r Rx

i-5sil

MS/

inte

gra-

guar

d R

este

k 10

Bo

th

141

Each

Ba

tch

034

Tent

ativ

e d

etec

ted

fu

ll sc

an

GC

M

SD

Q

EI

+ N

O

NO

YES

Agi

lent

597

3 M

SD

10

AC

N

DSP

E (P

SA/M

gSO

4)

HP-5

MS

10

Both

95

0

035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

44

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ETH

OX

IQU

IN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Con

firm

ed w

ith

seco

nd m

etho

d

1 4

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

G

C

MSD

Q

QQ

EI

+

YES

YES

N

O

Ther

mo

TSQ

Q

uant

um G

C

10

Ace

tone

/PE/

DC

M

Na2

SO4

RXi-5

SIL

MS

1 Bo

th

199

Each

Ba

tch

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.4

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.01

YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

45

ETR

IMFO

S

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

1.6

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

0.6

0.8

LC

M

SD

TOF

ESI

+ N

O

NO

N

A

YES

Bruk

er M

axis

10

EtO

Ac

Non

e A

ccla

im R

SLC

120

C

18, 2

,1*1

00 m

m

1 Bo

th

1000

Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 18

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1.3

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

0 N

O

Var

ian

320

50

Ace

tone

L/

L D

B5 ty

pe

8 Bo

th

146

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±0.5

%

GC

M

SD

Q

EI

+ YE

S YE

S 0.

010

mg/

kg

YES

Agi

lent

78

90-5

975C

15

A

CN

PS

A

HP-5

MS

10

Aut

o 21

1 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

46

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ETR

IMFO

S

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

EI

+

NO

YE

S 0.

010

NO

G

C-M

S/M

S (A

gile

nt)

15

AC

N

QuE

ChE

RS

DB

5MS

1 Bo

th

130

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl 5

%

phen

yl si

loxa

ne

2 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.01

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d

-0.2

3 -0

.04

isoto

pe

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

94

3 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2

G

C

FPD

YES

YES

0.01

N

O

Var

ian

3800

GC

10

A

CN

D

SPE

with

PSA

Rt

x-O

PP

1 Bo

th

302

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

47

ETR

IMFO

S

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Mat

ch w

ith

anal

ytic

al

stan

dar

d

(Ma

tch

927,

ra

nge

0-10

00)

GC

M

SD

TOF

EI

YE

S YE

S LO

Q: 2

pp

b

YES

GC

xGC

-TO

F M

S Pe

gasu

s 4D

10

A

CN

Q

uEC

hERS

w

ithou

t PSA

DB5

-MS

(30

m x

0,2

5 m

m x

0,2

5 µm

) in

the

1st D

imen

sion,

BP

X-50

(2 m

x 0

,1

mm

x 0

,1 µ

m) i

n th

e 2n

d D

imen

sion

10

Aut

o

029

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

IT

EI

+ YE

S YE

S 0.

01

YES

10

A

CN

N

O

DB-

5MS

5 Bo

th

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Ther

mo

TSQ

Q

uant

um X

LS

Ultra

10

A

CN

PS

A

Cap

illary

1

Both

15

0 A

lway

s

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.5

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01

YES

Agi

lent

GC

-MSD

78

90A

/597

5c

10

AC

N

PSA

, C18

HP

-5M

S 1

Aut

o 92

7

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o M

icro

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 5

Both

11

0 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5973

MSD

10

A

CN

D

SPE

HP-5

MSI

20

Bo

th

113

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

48

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ETR

IMFO

S

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


040

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 5

973

30

EtO

Ac

HPG

PC

DB-

5MS

2 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S

NO

TS

Q Q

uant

um

10

AC

N

QuE

ChE

RS

VF

5 M

S 3

Both

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

G

C

MSD

Q

QQ

EI

+

YES

YES

N

O

Ther

mo

TSQ

Q

uant

um G

C

10

Ace

tone

/PE/

DC

M

Na2

SO4

RXi-5

SIL

MS

1 Bo

th

199

Each

Ba

tch

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.4

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

3

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

39

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

120

0 LC

+646

0QQ

Q

10

AC

N

DSP

E YM

C T

riart

C18

2*

100

mm

3µm

5

Both

35

4 D

aily

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

5

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

49

FEN

PR

OP

IDIN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

NO

0.

01

YES

Agi

lent

597

3 in

ert

5 A

CN

HP-5

MSU

I 5

Both

Dai

ly

002

Con

firm

ed w

ith

seco

nd m

etho

d

0.2

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

1.2

1

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S N

O

NA

N

O

Agi

lent

646

0,

1290

HPLC

10

Et

OA

c N

one

Wa

ters

, HSS

T3,

15

0 x

2.1m

m

2 Bo

th

500

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 80

Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

13.8

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

(=RL

) N

O

API

5500

10

A

CN

D

SPE

Syne

rgie

Fus

ion

RP80

A

8 M

anua

l 35

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.8

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

50

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

FEN

PR

OP

IDIN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±0.5

%

GC

M

SD

Q

EI

+ YE

S YE

S 0.

010

mg/

kg

YES

Agi

lent

78

90-5

975C

15

A

CN

PS

A

HP-5

MS

10

Aut

o 21

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

TO

F EI

YES

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.15

0.

12

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

91

8 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

51

FEN

PR

OP

IDIN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

GC

+

320-

MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

274.

2>14

7.1,

27

4.2>

117.

0 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S LO

Q: 2

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

025-

0.25

µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

14

1 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-2.0

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.05

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

274.

3->1

47.1

, 27

4.3-

>86.

1 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410B

10

A

CN

D

SPE

C18

2

Both

18

7 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

52

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

FEN

PR

OP

IDIN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


040

Tent

ativ

e d

etec

ted

16

3

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1.2

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

cqui

ty B

EH

(100

x2.1

mm

i.d

.) 5

Both

23

0 Ea

ch B

atc

h

048

Con

firm

ed w

ith

seco

nd m

etho

d

3

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O T

Q

MS

10

AC

N

BE

H C

18 1

,7µm

3

Both

60

D

aily

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

38

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

120

0 LC

+646

0QQ

Q

10

AC

N

DSP

E YM

C T

riart

C18

2*

100

mm

3µm

5

Both

35

4 D

aily

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

53

FLU

FEN

AC

ET

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt 5

973

iner

t 5

AC

N

HP

-5 M

SUI

5 Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

3.1

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

-1.2

2.

2

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

Tent

ativ

e d

etec

ted

N

A

NA

LC

MSD

Q

QQ

ES

I +

YES

NO

N

A

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3.2

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

54

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

FLU

FEN

AC

ET

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, MS

API

30

00

10

AC

N

DSP

E (P

SA, M

gSO

4)

C18

3µ

50x2

mm

10

Bo

th

550

Alw

ays

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

1 -0

.35

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

90

5 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar

+320

-MS

10

AC

N

DSP

E w

ith P

SA

Rest

ek U

ltra

C18

10

Bo

th

302

Each

Ba

tch

028

Tent

ativ

e d

etec

ted

36

4.1>

152.

2,

364.

1>19

4.2

LC

MSD

Q

QQ

ES

I +

NO

N

O 1

0-10

0 pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o 59

1

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-1.3

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.05

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Con

firm

ed w

ith

seco

nd m

etho

d

full

scan

G

C

MSD

Q

EI

+

NO

N

O

YE

S A

gile

nt 5

973

MSD

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 10

Bo

th

950

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

55

FLU

FEN

AC

ET

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

040

Con

firm

ed w

ith

seco

nd m

etho

d

0 4

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

cqui

ty B

EH

(100

x2.1

mm

i.d

.) 5

Both

23

0 Ea

ch B

atc

h

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.01

YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

58

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

120

0 LC

+646

0QQ

Q

10

AC

N

DSP

E YM

C T

riart

C18

2*

100

mm

3µm

5

Both

35

4 D

aily

053

Tent

ativ

e d

etec

ted

12

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

56

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

FLU

TOLA

NIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

2.8

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

-1.2

1.

1

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

G

C

MSD

Q

QQ

EI

+

YES

NO

N

A

NO

Th

erm

o TS

Q

Qua

ntum

XLS

10

Et

OA

c N

one

Ther

mo

TG-5

SILM

S,

30m

*0.2

5mm

* 0.

25um

2

Aut

o 50

0 Ea

ch B

atc

h

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Tent

ativ

e d

etec

ted

1.3

LC

M

SD

Q-T

OF

ESI

+ N

O

NO

YES

5600

trip

le T

OF

10

AC

N

Non

e re

vers

ed p

hase

2

Aut

o 60

0 W

e d

o no

t ha

ve a

st

and

ard

009

Tent

ativ

e d

etec

ted

35

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

(=RL

) N

O

API

4000

10

A

CN

D

SPE

Syne

rgie

Fus

ion

RP80

A

8 M

anua

l 25

0

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

57

FLU

TOLA

NIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±0.5

%

GC

M

SD

Q

EI

+ YE

S YE

S 0.

010

mg/

kg

YES

Agi

lent

78

90-5

975C

15

A

CN

PS

A

HP-5

MS

10

Aut

o 21

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl

5% p

heny

l silo

xane

2

Aut

o

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

TO

F

YE

S YE

S 0.

01

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E Ph

enom

enen

x

ZB-5

MS

3 Bo

th

750

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.1

7 -0

.71

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

93

3 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

58

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

FLU

TOLA

NIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

028

Tent

ativ

e d

etec

ted

Mat

ch w

ith

NIS

T Lib

rary

(M

atc

h 82

8,

rang

e 0-

1000

)

GC

M

SD

TOF

EI

N

O

NO

10-

100

ppb

YE

S G

CxG

C-T

OF

MS

Pega

sus 4

D

10

AC

N

QuE

ChE

RS

with

out P

SA

DB5

-MS

(30

m x

0,2

5 m

m x

0,2

5 µm

) in

the

1st D

imen

sion,

BP

X-50

(2 m

x 0

,1

mm

x 0

,1 µ

m) i

n th

e 2n

d D

imen

sion

10

Aut

o 50

0

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

S/M

S Q

QQ

EI

+

YES

YES

0.02

5-0.

25

µg/m

l N

O

Wa

ters

Qua

ttro

Mic

ro G

C

10

EtO

Ac

Filte

r Rx

i-5sil

MS/

inte

gra-

guar

d R

este

k 10

Bo

th

141

Each

Ba

tch

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Ther

mo

TSQ

Q

uant

um X

LS

Ultra

10

A

CN

PS

A

Cap

illary

1

Both

15

0 A

lway

s

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-1.9

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.01

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5973

MSD

10

A

CN

D

SPE

HP-5

MSI

20

Bo

th

113

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 5

973

30

EtO

Ac

HPG

PC

DB-

5MS

2 A

uto

apro

x 50

0

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

59

FLU

TOLA

NIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S

NO

TS

Q Q

uant

um

10

AC

N

QuE

ChE

RS

VF

5 M

S 3

Both

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons +

io

n ra

tio

LC

MSD

Q

QQ

ES

I +

YES

YES

5-10

00

µg/k

g N

O

Wa

ters

Qua

ttro

Prem

ier X

E 15

A

ceto

ne/P

E/D

CM

N

O

Acq

uity

BEH

(1

00x2

.1 m

m i.

d.)

5 Bo

th

230

Each

Ba

tch

048

Con

firm

ed w

ith

seco

nd m

etho

d

6

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

9

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

60

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

IMA

ZA

PY

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I -

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410

10

AC

N

DSP

E Ec

lipse

XD

B-C

18

4 M

anua

l 13

9 Ea

ch B

atc

h

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

010

Tent

ativ

e d

etec

ted

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

BI40

00

10

AC

N

NO

C

18

55

Both

ap

rox

580

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E (P

SA, M

gSO

4)

C18

3µ

50x2

mm

10

Bo

th

550

Alw

ays

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT ES

I -

YES

YES

0.01

N

O

10

A

CN

Both

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

262.

2>21

7.0,

26

2.2>

149.

0 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S LO

Q:

2 pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.1

m

m, 5

µm

2

Aut

o

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

034

Tent

ativ

e d

etec

ted

5

trans

ition

s LC

QQ

Q

ESI

+ N

O

NO

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

A

CN

D

SPE

(PSA

/MgS

O4)

RP

-18

end

capp

ed

5 Bo

th

500

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

040

Tent

ativ

e d

etec

ted

2

0

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

61

IMA

ZA

PY

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

20

Aut

o 14

3

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1.1

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

A

CN

D

SPE(

PSA

) Lu

na C

18

5 Bo

th

350

Dai

ly

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

62

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

IOX

YN

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

- YE

S N

O

NA

N

O

Agi

lent

646

0,

1290

HPLC

10

Et

OA

c N

one

Wa

ters

, HSS

T3,

150

x

2.1m

m

2 Bo

th

500

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I -

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

3 A

uto

300

Each

Ba

tch

009

Tent

ativ

e d

etec

ted

2

trans

ition

s LC

QQ

Q

ESI

- N

O

NO

NO

A

PI40

00

10

AC

N

DSP

E Sy

nerg

ie F

usio

n RP

80A

8

Man

ual

40

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

0.02

N

O

ABI

4000

10

A

CN

N

O

C18

55

Bo

th

apro

x 58

0 A

lway

s

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, MS

A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT ES

I -

YES

YES

0.01

N

O

10

A

CN

Both

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

63

IOX

YN

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d

-0.0

2 0.

9 iso

tope

LC

M

SD

Orb

itra

p

ESI

- N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

91

0 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

369.

6>12

6.9,

36

9.6>

214.

8 LC

M

SD

QQ

Q

ESI

- YE

S YE

S LO

Q: 2

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

- YE

S YE

S 0.

005-

0.04

µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

5 Et

OA

c Fil

ter

HSS

T3

2 Bo

th

250

Each

Ba

tch

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I -

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

- YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

040

Con

firm

ed w

ith

seco

nd m

etho

d

9 3

LC

TOF

ESI

- N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T G

-64

10A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

80

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3.6

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

- N

O

NO

5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

lltim

a C

18

(150

x3 m

m i.

d.)

5 Bo

th

27

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

64

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

IOX

YN

IL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.8

LC

MSD

Q

QQ

ES

I -

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

A

CN

D

SPE(

PSA

) Lu

na C

18

5 Bo

th

350

Dai

ly

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O T

Q

MS

10

AC

N

BE

H C

18 1

,7µm

3

Both

60

D

aily

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.01

7

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

7 D

aily

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

65

ISO

PR

OTU

RO

N

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

API

4000

10

A

CN

N

one

C18

5

Man

ual

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

-1.2

2.

2

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410

10

AC

N

DSP

E Ec

lipse

XD

B-C

18

4 M

anua

l 13

9 Ea

ch B

atc

h

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

28

.8

2

trans

ition

s LC

QQ

Q

ESI

+ YE

S YE

S 0.

01 (=

RL)

NO

A

PI40

00

10

AC

N

DSP

E Sy

nerg

ie F

usio

n RP

80A

8

Man

ual

250

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

ABI

4000

10

A

CN

N

O

C18

55

Bo

th

apro

x 58

0 A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

NO

32

00q

trap

10

A

CN

PS

A

T-3

5 M

anua

l 17

0 1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

66

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ISO

PR

OTU

RO

N

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

TO

F EI

YES

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S

NO

A

gile

nt 6

490

15

AC

N

PSA

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

0.

64

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

67

ISO

PR

OTU

RO

N

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar

+320

-MS

10

AC

N

DSP

E w

ith P

SA

Rest

ek U

ltra

C18

10

Bo

th

302

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

207.

2>72

.1,

207.

2>13

4.2

LC

MSD

Q

QQ

ES

I +

YES

YES

LOQ

: 2

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o

029

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.12

5 µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

207.

1->7

2.0,

20

7.1-

>165

.1

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

641

0B

10

AC

N

DSP

E C

18

2 Bo

th

187

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

68

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

ISO

PR

OTU

RO

N

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


040

Con

firm

ed w

ith

seco

nd m

etho

d

3 2

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

20

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

044

Tent

ativ

e d

etec

ted

LC

Q

QQ

EI

+

YES

A

gile

nt 6

410

10

AC

N

Zo

rbax

SB

C-1

8 5

Aut

o

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Tent

ativ

e d

etec

ted

2

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.9

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

A

CN

D

SPE(

PSA

) Lu

na C

18

5 Bo

th

350

Dai

ly

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O

TQ M

S 10

A

CN

BEH

C18

1,7

µm

3 Bo

th

60

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.0

55

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

120

0 LC

+646

0QQ

Q

10

AC

N

DSP

E YM

C T

riart

C18

2*

100

mm

3µm

5

Both

35

4 D

aily

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

69

MET

AZ

AC

HLO

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt 5

973

iner

t 5

AC

N

HP

-5 M

SUI

5 Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

3.1

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Ther

mo

TSQ

Q

uant

um X

LS

10

EtO

Ac

Non

e Th

erm

o TG

-5SI

LMS,

30

m*0

.25m

m*

0.25

um

2 A

uto

500

Each

Ba

tch

Con

firm

ed w

ith

seco

nd m

etho

d

-0.6

2.

4

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

36

.6

2

trans

ition

s LC

QQ

Q

ESI

+ YE

S YE

S 0.

01 (=

RL)

NO

A

PI40

00

10

AC

N

DSP

E Sy

nerg

ie F

usio

n RP

80A

8

Man

ual

250

Sche

dul

ed

MRM

M

etho

d

also

use

d

for

qua

ntifi

catio

n

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.3

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

70

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

MET

AZ

AC

HLO

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±0.5

%

GC

M

SD

Q

EI

+ YE

S YE

S 0.

010

mg/

kg

YES

Agi

lent

78

90-5

975C

15

A

CN

PS

A

HP-5

MS

10

Aut

o 21

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl

5% p

heny

l silo

xane

2

Aut

o

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3x

SIM

mas

ses

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01

YES

Agi

lent

597

5 10

A

CN

PS

A

GsB

P-5M

S 5

Both

50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d

-0.1

9 -0

.43

isoto

pe

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

84

0 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

71

MET

AZ

AC

HLO

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 4

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

G

C +

320

-MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

028

Con

firm

ed w

ith

seco

nd m

etho

d

278.

2>14

3.2,

27

8.2>

210.

2 LC

M

SD

QQ

Q

ESI

+ N

O

NO

10-

100

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o 59

1

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

YE

S V

aria

n 32

0 15

A

CN

C18

10

A

uto

150

Each

Ba

tch

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

S/M

S Q

QQ

EI

+

YES

YES

0.00

5-0.

4 µg

/ml

NO

W

ate

rs Q

uattr

o M

icro

GC

10

Et

OA

c Fil

ter

Rxi-5

sil M

S/in

tegr

a-gu

ard

Res

tek

10

Both

37

3 Ea

ch B

atc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-2.1

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.05

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Con

firm

ed w

ith

seco

nd m

etho

d

7 3

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

72

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

MET

AZ

AC

HLO

R

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

20

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S

NO

TS

Q Q

uant

um

10

AC

N

QuE

ChE

RS

VF

5 M

S 3

Both

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.2

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

053

Tent

ativ

e d

etec

ted

9

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

73

NA

PR

OP

AM

IDE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt 5

973

iner

t 5

AC

N

HP

-5 M

SUI

5 Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

4.2

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

-0.6

0.

9

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 18

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

5.4

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

74

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

NA

PR

OP

AM

IDE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl

5% p

heny

l silo

xane

2

Aut

o

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

96

4 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

8 1.

85

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

GC

+

320-

MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

75

NA

PR

OP

AM

IDE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


028

Con

firm

ed w

ith

seco

nd m

etho

d

272.

1>12

9.3,

27

2.1>

171.

1 LC

M

SD

QQ

Q

ESI

+ N

O

NO

10-

100

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o 59

1

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

GC

QQ

Q

EI

+ YE

S YE

S 0.

02

NO

V

aria

n 45

0 15

A

ceto

ne

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.12

5 µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

m

in 3

ions

G

C

MSD

Q

EI

+

YES

NO

0.

01

YES

Agi

lent

GC

-MSD

78

90A

/597

5c

10

AC

N

PSA

, C18

HP

-5M

S 1

Aut

o 92

7

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Con

firm

ed w

ith

seco

nd m

etho

d

11

3

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

76

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

NA

PR

OP

AM

IDE

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

3

G

C

MSD

TO

F EI

YES

YES

0.01

YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O T

Q

MS

10

AC

N

BE

H C

18 1

,7µm

3

Both

60

D

aily

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.01

7

Qio

n ra

tio

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

68

90G

C+5

975M

S 10

A

CN

D

SPE

REST

EK-5

MS

50

Both

16

8 D

aily

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

77

PR

OM

ETR

YN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt 5

973

iner

t 5

AC

N

HP

-5 M

SUI

5 Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

5.3

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

3 0.

9

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 18

0 Ea

ch B

atc

h

010

Tent

ativ

e d

etec

ted

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

BI40

00

10

AC

N

NO

C

18

55

Both

ap

rox

580

Alw

ays

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

4.7

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

78

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

PR

OM

ETR

YN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.01

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

91

7 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

Con

firm

ed w

ith

seco

nd m

etho

d

0.28

1.

2 iso

tope

, 2 io

ns

< 5p

pm

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

GC

+

320-

MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

79

PR

OM

ETR

YN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


028

Con

firm

ed w

ith

seco

nd m

etho

d

242.

2>20

0.1,

24

2.2>

158.

1 LC

M

SD

QQ

Q

ESI

+ N

O

NO

10-

100

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o 59

1

029

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.12

5 µg

/ml

NO

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5

m

in 3

ions

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o M

icro

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 5

Both

11

0 Ea

ch B

atc

h

035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5973

MSD

10

A

CN

D

SPE

HP-5

MSI

20

Bo

th

113

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

80

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

PR

OM

ETR

YN

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


040

Con

firm

ed w

ith

seco

nd m

etho

d

30

3

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

G

C

MSD

Q

QQ

EI

+

YES

YES

N

O

Ther

mo

TSQ

Q

uant

um G

C

10

Ace

tone

/PE/

DC

M

Na2

SO4

RXi-5

SIL

MS

1 Bo

th

199

Each

Ba

tch

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Each

Ba

tch

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O T

Q

MS

10

AC

N

BE

H C

18 1

,7µm

3

Both

60

D

aily

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.05

4

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

354

Dai

ly

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

2

3

SIM

Ions

G

C

MSD

Q

EI

+

NO

N

O

>0.0

5 m

g/kg

YE

S Th

erm

o D

SQ

10

DC

M

Dia

tom

aceo

us

earth

1 Bo

th

400

Ever

y 6

Mon

ths

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

81

PR

OP

AQ

UIZ

AFO

P

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

1.2

3.7

LC

M

SD

TOF

ESI

+ N

O

NO

N

A

YES

Bruk

er M

axis

10

EtO

Ac

Non

e A

ccla

im R

SLC

120

C

18, 2

,1*1

00 m

m

1 Bo

th

1000

Ea

ch B

atc

h

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410

10

AC

N

DSP

E Ec

lipse

XD

B-C

18

4 M

anua

l 13

9 Ea

ch B

atc

h

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

Q-T

OF

ESI

+ N

O

NO

0.

01

Br

uker

Max

is 10

A

CN

Both

70

0 Ea

ch B

atc

h

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

028

Tent

ativ

e d

etec

ted

44

4.1>

299.

1,

444.

1>10

0.0

LC

MSD

Q

QQ

ES

I +

NO

N

O 1

0-10

0 pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o 59

1

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

YE

S V

aria

n 32

0 15

A

CN

C18

10

A

uto

150

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

82

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

PR

OP

AQ

UIZ

AFO

P

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

034

Tent

ativ

e d

etec

ted

3

trans

ition

s LC

QQ

Q

ESI

+ N

O

NO

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

A

CN

D

SPE

(PSA

/MgS

O4)

RP

-18

end

capp

ed

5 Bo

th

500

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

444.

1->1

00.1

, 44

4.1-

>299

.1

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

641

0B

10

AC

N

DSP

E C

18

2 Bo

th

187

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

4 5

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.3

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

A

CN

D

SPE(

PSA

) Lu

na C

18

5 Bo

th

350

Dai

ly

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O

TQ

MS

10

AC

N

BE

H C

18 1

,7µm

3

Both

60

D

aily

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

83

PY

RIF

ENO

X

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

3.0

and

3.

9

G

C

MSD

Q

EI

+

YES

YES

not

valid

ated

YE

S A

T 59

75

10

AC

N

SPE

HP5-

MS

10

Aut

o ap

rox

750

Alw

ays

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Con

firm

ed w

ith

seco

nd m

etho

d

3 0.

6

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

3 Bo

th

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 18

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

84

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

PY

RIF

ENO

X

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 10

N

O

Agi

lent

689

0 15

A

ceto

ne/P

E/D

CM

N

one

95%

met

hyl

5% p

heny

l silo

xane

2

Aut

o

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, M

S A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

G

C

MSD

TO

F

YE

S YE

S 0.

01

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E Ph

enom

enen

x

ZB-5

MS

3 Bo

th

750

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.01

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Con

firm

ed w

ith

seco

nd m

etho

d

-0.1

6 0.

22

isoto

pe, t

wo

isom

er p

eaks

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

91

6 sp

ectru

m, t

wo

isom

er p

eaks

G

C

MSD

TO

F EI

+

YES

YES

0.01

-0.1

YE

S Le

co P

egas

us IV

10

A

CN

D

SPE

(PSA

) RT

X-C

L pe

st

10

Aut

o 55

7 Ea

ch B

atc

h

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar

+320

-MS

10

AC

N

DSP

E w

ith P

SA

Rest

ek U

ltra

C18

10

Bo

th

302

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

297.

1>93

.1,

295.

1>92

.9

LC

MSD

Q

QQ

ES

I +

YES

YES

LOQ

: 8

ppb

N

O

LC: A

gile

nt 1

200,

M

S: A

PI 4

000

QTR

AP

10

AC

N

QuE

ChE

RS

with

out P

SA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

85

PY

RIF

ENO

X

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.8

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.01

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.02

YE

S HP

5973

MSD

10

A

CN

D

SPE

HP-5

MSI

20

Bo

th

113

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

2 4

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 sc

an

GC

M

SD

IT EI

YES

YES

0.01

0 YE

S V

aria

n Sa

turn

40

00

10

AC

N

DSP

E V

aria

n V

F 1

Aut

o 26

0 D

aily

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

86

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

PY

RIF

ENO

X

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

12

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

cqui

ty B

EH

(100

x2.1

mm

i.d

.) 5

Both

23

0 Ea

ch B

atc

h

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

Con

firm

ed w

ith

seco

nd m

etho

d

0

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

87

SP

INO

SA

D

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

API

4000

10

A

CN

N

one

C18

5

Man

ual

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

006

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

<2

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.010

m

g/kg

N

O

Wa

ters

qua

ttro

prem

ier

15

AC

N

Non

e BE

H C

18

10

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410

10

AC

N

DSP

E Ec

lipse

XD

B-C

18

4 M

anua

l 13

9 Ea

ch B

atc

h

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

ABI

4000

10

A

CN

N

O

C18

55

Bo

th

apro

x 58

0 A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

NO

32

00q

trap

10

A

CN

PS

A

T-3

5 M

anua

l 17

0 1

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

88

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

SP

INO

SA

D

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



017

Tent

ativ

e d

etec

ted

LC

MSD

Q

QQ

ES

I

NO

N

O

Agi

lent

641

0 15

A

ceto

ne/P

E/D

CM

N

O

C-1

8 3

Both

018

Tent

ativ

e d

etec

ted

5

5 ac

cura

te

mas

s LC

O

rbitr

ap

O

rbitr

ap

ES

I +

YES

YES

0.01

- 0.

05

mg/

kg

YES

Ther

mo

Exac

tive

10

AC

N

PSA

C

18

5 Bo

th

120

Alw

ays

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

021

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

15

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

HP

LC A

gile

nt

1100

, MS

A

PI 3

000

10

AC

N

DSP

E

(PSA

, MgS

O4)

C

18 3

µ 50

x2m

m

10

Both

55

0 A

lway

s

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.2

7 1.

3 iso

tope

, 2 io

ns

< 5p

pm

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Tent

ativ

e d

etec

ted

0.

22

1.4

othe

r sp

inos

yns

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 2.

5 %

2.

5 tra

nsiti

on 1

an

d 2

LC

M

SD

Q-T

RAP

ESI

+ YE

S YE

S 0.

01

YES

3200

Qtra

p

10

AC

N

DSP

E C

18

50

Aut

o 52

1 Ev

ery

Wee

k

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3 0.

7 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

V

aria

n Pr

o St

ar

+320

-MS

10

AC

N

DSP

E w

ith P

SA

Rest

ek U

ltra

C18

10

Bo

th

302

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

732.

6>14

2.2,

73

2.6>

98.2

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S LO

Q: 8

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2

.1 m

m, 5

µm

2

Aut

o

029

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

89

SP

INO

SA

D

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

Non

e N

one

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

D

SPE

Wa

ters

-C18

2,

1x50

mm

x1,7

‚µm

5

Aut

o 60

0 Ev

ery

Wee

k

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

732.

4->1

42.0

, 73

2.4-

>98.

1,

746.

5->1

42.1

, 74

6.5-

>98.

1

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

641

0B

10

AC

N

DSP

E C

18

2 Bo

th

187

Each

Ba

tch

040

Con

firm

ed w

ith

seco

nd m

etho

d

1 7

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

20

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

90

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

SP

INO

SA

D

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s +

ion

ratio

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 5-

1000

µg

/kg

NO

W

ate

rs Q

uattr

o Pr

emie

r XE

15

Ace

tone

/PE/

DC

M

NO

A

cqui

ty B

EH

(100

x2.1

mm

i.d

.) 5

Both

23

0 Ea

ch B

atc

h

048

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1.2

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 N

O

Agi

lent

641

0 10

A

CN

D

SPE(

PSA

) Lu

na C

18

5 Bo

th

350

Dai

ly

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O

TQ M

S 10

A

CN

BEH

C18

1,7

µm

3 Bo

th

60

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.07

8

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

354

Dai

ly

051

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.05

ABS

ciex

API

200

0 10

A

CN

PS

A

wat

ers A

tlant

is 5

Aut

o 11

7 Ea

ch B

atc

h

053

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 M

RM

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S >0

.005

m

g/kg

N

O

API

4000

10

A

CN

PS

A

10

Bo

th

180

Ever

y M

onth

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

91

TER

BA

CIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S A

gile

nt 5

973

iner

t 5

AC

N

HP

-5 M

SUI

5 Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

8.0

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I -

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Tent

ativ

e d

etec

ted

5

GC

M

SD

TOF

EI

N

O

NO

YES

GC

T M

icro

mas

s 12

.5

EtO

Ac

GPC

ca

pilla

ry

1 A

uto

NIS

T lib

rary

W

e d

o no

t ha

ve a

st

and

ard

009

Tent

ativ

e d

etec

ted

2

trans

ition

s G

C

MSD

Q

QQ

EI

+

NO

N

O

N

O

Ther

mo

TSQ

Q

uant

um

10

AC

N

DSP

E TG

-5M

S 30

m

2 M

anua

l 18

0 Ea

ch B

atc

h

010

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.7

2

trans

ition

s G

C

MSD

Q

EI

+

YES

YES

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

- YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

92

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

TER

BA

CIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

QQ

EI

YES

YES

0.01

N

O

agile

nt

10

AC

N

DSP

E HP

5MS

1

200

Alw

ays

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

IT ES

I -

YES

YES

0.01

N

O

10

A

CN

Both

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I -

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.3

1.

7 iso

tope

, 2 io

ns

< 5p

pm

LC

MSD

O

rbitr

ap

ES

I +

NO

N

O

0.01

-0.1

YE

S Ex

activ

e 10

A

CN

N

one

C18

Atla

ntis

T3

5 Bo

th

570

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

93

9 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

026

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

4 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

GC

+

320-

MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

028

Tent

ativ

e d

etec

ted

Mat

ch w

ith

NIS

T Lib

rary

(M

atc

h 92

5,

rang

e 0-

1000

)

GC

M

SD

TOF

EI

N

O

NO

10-

100

ppb

YE

S G

CxG

C-T

OF

MS

Pega

sus 4

D

10

AC

N

QuE

ChE

RS

with

out P

SA

DB5

-MS

(30

m x

0,2

5 m

m x

0,2

5 µm

) in

the

1st D

imen

sion,

BP

X-50

(2 m

x 0

,1

mm

x 0

,1 µ

m) i

n th

e 2n

d D

imen

sion

10

Aut

o 50

0

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

GC

QQ

Q

EI

+ N

O

NO

0.

02

NO

V

aria

n 45

0 15

A

ceto

ne

V

5MS

1 A

uto

150

Each

Ba

tch

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

93

TER

BA

CIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-4.1

min

3 io

ns

GC

M

SD

Q

EI

+ YE

S N

O

0.01

YE

S A

gile

nt G

C-M

SD

7890

A/5

975c

10

A

CN

PS

A, C

18

HP-5

MS

1 A

uto

927

034

Con

firm

ed w

ith

seco

nd m

etho

d

full

scan

G

C

MSD

Q

EI

+

NO

N

O

YE

S A

gile

nt 5

973

MSD

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 10

Bo

th

950

035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

036

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

10

AC

N

5 A

uto

039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Con

firm

ed w

ith

seco

nd m

etho

d

17

8

LC

TO

F ES

I -

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

043

Tent

ativ

e d

etec

ted

0

0 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

YES

Api

320

0QT

10

AC

N

DSP

E Ph

enom

enex

fusio

n 10

A

uto

200

Dai

ly

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

G

C

MSD

Q

QQ

EI

+

YES

YES

N

O

Ther

mo

TSQ

Q

uant

um G

C

10

Ace

tone

/PE/

DC

M

Na2

SO4

RXi-5

SIL

MS

1 Bo

th

199

Each

Ba

tch

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.7

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

6

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

94

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

TER

BA

CIL

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S

NO

W

ate

rs Q

uattr

o m

icro

GC

10

A

CN

DB-

5MS

3 Bo

th

150

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.03

6

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

-0.0

5 YE

S A

gile

nt 1

200

LC+6

460Q

QQ

10

A

CN

D

SPE

YMC

Tria

rt C

18

2*10

0 m

m 3

µm

5 Bo

th

354

Dai

ly

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

12

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

95

TER

BU

MET

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

5.0

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

004

Tent

ativ

e d

etec

ted

N

A

NA

LC

MSD

Q

QQ

ES

I +

YES

NO

N

A

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

-1.2

0.

6

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

007

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1 N

one

G

C

MSD

Q

EI

+

YES

YES

0.01

N

O

Agi

lent

68

90/5

973

10

AC

N

DSP

E HP

-5M

S 2

Man

ual

183

Each

Ba

tch

008

Tent

ativ

e d

etec

ted

0.1

LC

M

SD

Q-T

OF

ESI

+ N

O

NO

YES

5600

trip

le T

OF

10

AC

N

Non

e re

vers

ed p

hase

2

Aut

o 60

0 W

e d

o no

t ha

ve a

st

and

ard

010

Tent

ativ

e d

etec

ted

3.

8

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S N

O

0.01

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

011

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

NA

G

C

MSD

Q

EI

+

NO

N

O

NA

YE

S 57

90 m

sd

10

AC

N

PSA

HP

-5M

S 20

A

uto

600

apro

x 0-

1

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

GC

QQ

Q

EI

+ YE

S YE

S 0.

01

NO

70

00B

10

AC

N

PSA

D

B-5M

S UI

2

Both

44

0

016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

018

Tent

ativ

e d

etec

ted

RT

lo

ckin

g

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01 -

0.05

m

g/kg

YE

S A

gile

nt M

SD

5975

B 10

A

CN

PS

A

HP5

10

Both

>

600

Alw

ays

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

96

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

TER

BU

MET

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

PI 5

500

10

AC

N

Pu

rsui

t XRs

Ultr

a

3 Bo

th

250

Each

Ba

tch

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

3

mas

ses

GC

M

SD

IT EI

+

YES

YES

0.05

YE

S V

aria

n Sa

turn

20

00

10

AC

N

PSA

V

acto

rFou

r 5 M

S 5

Aut

o 50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.1

6 -1

.5

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

75

5 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 0.

5 %

2.

5

GC

M

SD

ion

trap

EI

YES

YES

0.01

YE

S Tr

ap 4

000

- V

aria

n 10

A

CN

D

SPE

5%

1 µL

A

uto

450

Ever

y W

eek

027

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3 0.

7 3

trans

ition

s G

C

MSD

Q

QQ

EI

+

YES

YES

0.01

N

O

Var

ian

3800

GC

+

320-

MS

10

AC

N

DSP

E w

ith P

SA

VF-

1ms

4 Bo

th

302

Each

Ba

tch

028

Tent

ativ

e d

etec

ted

22

6.0>

170.

0,

226.

0>11

4.0

LC

MSD

Q

QQ

ES

I +

NO

N

O 1

0-10

0 pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o 59

1

029

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

NO

N

O

10

A

CN

N

O

Xter

ra C

18

20

Both

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

033

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.3

m

in 3

ions

G

C

MSD

Q

EI

+

YES

NO

0.

01

YES

Agi

lent

GC

-MSD

78

90A

/597

5c

10

AC

N

PSA

, C18

HP

-5M

S 1

Aut

o 92

7

034

Con

firm

ed w

ith

seco

nd m

etho

d

full

scan

G

C

MSD

Q

EI

+

NO

N

O

YE

S A

gile

nt 5

973

MSD

10

A

CN

D

SPE

(PSA

/MgS

O4)

HP

-5M

S 10

Bo

th

950

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

97

TER

BU

MET

ON

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software



035

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

G

C

MSD

Q

EI

NO

N

O

YE

S A

gile

nt 6

890N

10

A

CN

D

SPE

DB-

5 2

Aut

o

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Tent

ativ

e d

etec

ted

GC

M

SD

Q

EI

+ N

O

NO

YES

HP59

73 M

SD

10

AC

N

DSP

E HP

-5M

SI

20

Both

62

4 N

o st

and

ard

us

ed

040

Con

firm

ed w

ith

seco

nd m

etho

d

17

3

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

Tent

ativ

e d

etec

ted

3

LC

TO

F ES

I +

NO

N

O

YE

S A

gile

nt 6

230

10

AC

N

Non

e Ec

lipse

C18

3

Aut

o ap

rox

500

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.5%

2 tra

nsiti

ons

GC

M

SD

QQ

Q

EI

YE

S YE

S 0.

005

mg/

kg

NO

V

ARI

AN

CP-

3800

M

S-32

0 10

A

CN

PS

A

VF-

5MS

1 A

uto

210

045

Tent

ativ

e d

etec

ted

1

1 un

it

GC

M

SD

Q

EI

YE

S N

O

0.01

ppm

YE

S A

gile

nt 5

973

10

AC

N

PSA

HP

5 M

S UI

2

Aut

o 92

3 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.2

Sp

ectru

m

mat

ch

(reve

rsed

) G

C

MSD

IT

EI

+ YE

S YE

S 20

-10.

000

µg/k

g YE

S V

aria

n Sa

turn

20

00

15

Ace

tone

/PE/

DC

M

NO

V

F-5-

ms

5 Bo

th

550

Qua

rterly

048

Con

firm

ed w

ith

seco

nd m

etho

d

4

G

C

MSD

TO

F EI

YES

YES

0.00

5 YE

S Pe

gasu

s IV

10

A

CN

D

SPE(

PSA

) HP

-5M

S 5

Both

65

0 W

eekl

y

049

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

XEV

O

TQ M

S 10

A

CN

BEH

C18

1,7

µm

3 Bo

th

60

Dai

ly

050

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.03

2

Qio

n ra

tio

GC

M

SD

Q

EI

+ YE

S YE

S 0.

01-0

.05

YES

Agi

lent

68

90G

C+5

975M

S 10

A

CN

D

SPE

REST

EK-5

MS

50

Both

16

8 D

aily

051

Tent

ativ

e d

etec

ted

0.5

qual

ifier

s G

C

MSD

IT

EI

N

O

NO

YES

varia

n G

CM

S 40

00

10

AC

N

PSA

va

rian

fact

or fo

ur

5 Bo

th

053

Tent

ativ

e d

etec

ted

10

3 SI

M Io

ns

GC

M

SD

Q

EI

+ N

O

NO

>0

.05

mg/

kg

YES

Ther

mo

DSQ

10

D

CM

D

iato

mac

eous

ea

rth

1

Both

40

0 Ev

ery

6 M

onth

s

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

98

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

VA

MID

OTH

ION

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


001

Con

firm

ed w

ith

seco

nd m

etho

d

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

Agi

lent

649

0 5

AC

N

RP

-C18

10

Bo

th

D

aily

002

Con

firm

ed w

ith

seco

nd m

etho

d

8.4

GC

M

SD

Q

EI

+ YE

S YE

S no

t va

lidat

ed

YES

AT

5975

10

A

CN

SP

E HP

5-M

S 10

A

uto

apro

x 75

0 A

lway

s

002

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

API

4000

10

A

CN

N

one

C18

5

Man

ual

003

Con

firm

ed w

ith

seco

nd m

etho

d

0.05

5

2 tra

nsiti

ons

LC

Q

-TO

F ES

I +

NO

N

O

YE

S Br

uker

Max

is 10

A

CN

PS

A

RSLC

C18

1

Both

ap

rox

400

004

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

460,

12

90HP

LC

10

EtO

Ac

Non

e W

ate

rs, H

SS T

3,

150

x 2.

1mm

2

Both

50

0 Ea

ch B

atc

h

Con

firm

ed w

ith

seco

nd m

etho

d

-0.6

2.

4

LC

MSD

TO

F ES

I +

NO

N

O

NA

YE

S Br

uker

Max

is 10

Et

OA

c N

one

Acc

laim

RSL

C 1

20

C18

, 2,1

*100

mm

1

Both

10

00

Each

Ba

tch

006

Tent

ativ

e d

etec

ted

<1

3 d

iagn

ostic

io

ns

GC

M

SD

Q

EI

+ YE

S YE

S >0

.010

m

g/kg

YE

S Tr

ace

DSQ

15

A

CN

PS

A/C

18

DB5

MS

0.8

Both

008

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

1

2 tra

nsiti

ons

+acc

urat

e m

ass

LC

MSD

Q

-TRA

P ES

I +

YES

NO

0.

01

NO

Q

Trap

550

0 10

A

CN

N

one

reve

rsed

pha

se

2.5

Aut

o 30

0 Ea

ch B

atc

h

010

Tent

ativ

e d

etec

ted

6.

5

2 tra

nsiti

ons

GC

M

SD

Q

EI

+ YE

S N

O

YE

S HP

5975

C

10

AC

N

DSP

E HP

5MS

10

Both

ap

rox

1000

A

lway

s

012

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.6

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

W

ate

rs Q

uattr

o Pr

emie

r 10

M

etha

nol

NO

C

18

5 Bo

th

211

Alw

ays

013

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

4 N

A

ion

ratio

- qu

antif

ier

288/

146

qual

ifier

28

8/11

8

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

0 m

g/Kg

N

O

API

320

0 Q

TRA

P 10

.0

AC

N

d-S

PE

C18

20

M

anua

l 12

0 Ea

ch B

atc

h

014

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

±2.5

%

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

010

mg/

kg

YES

Wa

ters

-TQ

D

15

AC

N

PSA

UP

LC-B

EH C

18

10

Aut

o 33

1 Ea

ch B

atc

h

015

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

NA

N

A

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

0.01

N

O

6460

10

A

CN

PS

A

C18

-XB

2 Bo

th

440

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

Fina

l Rep

ort -

EUR

L-FV

-SM

-04,

201

2

99

VA

MID

OTH

ION

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


016

Con

firm

ed w

ith

seco

nd m

etho

d

MSD

Q

QQ

C

I +

YES

YES

0.00

5 N

O

LC-M

S/M

S (W

ate

rs)

15

AC

N

QuE

ChE

RS

C18

10

Bo

th

370

Alw

ays

017

Tent

ativ

e d

etec

ted

GC

M

SD

TOF

EI

N

O

NO

YES

LEC

O P

EGA

SUS

15

Ace

tone

/PE/

DC

M

NO

D

B-5

1 Bo

th

019

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

3

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

10

NO

A

gile

nt 6

490

15

AC

N

PSA

C

18

5 A

uto

020

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

bSci

ex

10

AC

N

DSP

E C

18

5 A

uto

200

Alw

ays

022

Tent

ativ

e d

etec

ted

0.

5 0.

05

LC

M

SD

TOF

ESI

+ YE

S YE

S

YES

LCT

PREM

IER

XE

15

MIN

I LUK

E N

O

C-1

8 7

Aut

o 34

3 Ev

ery

Da

y

023

Con

firm

ed w

ith

seco

nd m

etho

d

LC

Q-T

OF

ESI

+ N

O

NO

0.

01

Br

uker

Max

is 10

A

CN

Both

70

0 Ea

ch B

atc

h

024

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0.1

2

x M

RM

LC

MSD

Q

QQ

ES

I +

YES

YES

0.01

N

O

AB

Scie

x A

PI

4000

10

A

CN

PS

A

Phen

omen

ex C

18

10

Both

50

0 D

aily

025

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

-0.1

2 0.

76

isoto

pe, 2

ions

<

5ppm

LC

M

SD

Orb

itra

p

ESI

+ N

O

NO

0.

01-0

.1

YES

Exac

tive

10

AC

N

Non

e C

18 A

tlant

is T3

5

Both

57

0 Ea

ch B

atc

h

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

< 20

90

1 sp

ectru

m

GC

M

SD

TOF

EI

+ YE

S YE

S 0.

01-0

.1

YES

Leco

Peg

asus

IV

10

AC

N

DSP

E (P

SA)

RTX-

CL

pest

10

A

uto

557

Each

Ba

tch

028

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

288.

1>11

8.0,

28

8.1>

146.

0 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S LO

Q: 2

pp

b

NO

LC

: Agi

lent

120

0,

MS:

API

400

0 Q

TRA

P 10

A

CN

Q

uEC

hERS

w

ithou

t PSA

Supe

lco

Disc

over

y C

18, 1

50 m

m x

2.

1 m

m, 5

µm

2

Aut

o

030

Tent

ativ

e d

etec

ted

LC

Q

QQ

ES

I +

YES

YES

0.02

N

O

Var

ian

320

15

AC

N

C

18

10

Aut

o 15

0 Ea

ch B

atc

h

APP

ENDI

X 3.

Met

hods

use

d by

par

ticip

ants

for d

etec

ting

pest

icid

es.

100

Fi

nal R

epor

t - E

URL-

FV-S

M-0

4, 2

012

VA

MID

OTH

ION

Laboratory Code



MS Tolerance (ppm)



Detector

Analyzer

IonizationMode

Polarity

Routine Method?

Routine Scope?


Full Scan

Instrument Model

Sample Weight (g)

Extraction Solvent

Clean up Step

Column Type


Software


(pesticides ONLY)


031

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

005-

0.4

µg/m

l N

O

UPLC

-MSM

S (W

ate

rs A

quity

UP

LC sy

stem

, A

PI 5

000

Trip

elqu

adro

pol,

Scie

x

10

EtO

Ac

Filte

r HS

S T3

2

Both

37

3 Ea

ch B

atc

h

032

Tent

ativ

e d

etec

ted

0

2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

W

ate

rs A

cqui

ty

TQD

10

M

etha

nol

Filte

r C

18

6 A

uto

150

Alw

ays

034

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

Q

QQ

ES

I +

YES

YES

N

O

Wa

ters

Qua

ttro

Prem

ier

10

AC

N

DSP

E (P

SA/M

gSO

4)

RP-1

8 en

dca

pped

5

Both

18

6 Ea

ch B

atc

h

036

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

10

AC

N

5 A

uto

350

037

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MS/

MS

QQ

Q

ESI

+ YE

S YE

S 0.

010

NO

40

00 Q

TRA

P 10

A

CN

D

SPE

C18

hyd

ro

Phen

omen

ex

40

Man

ual

A

lway

s

038

Tent

ativ

e d

etec

ted

N

one

Non

e 2

trans

ition

s LC

M

SD

QQ

Q

ESI

+ N

O

NO

NO

A

PI 4

000

10

AC

N

DSP

E W

ate

rs-C

18

2,1x

50m

mx1

,7‚µ

m

5 A

uto

600

Ever

y W

eek

039

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

288.

1->1

46.1

, 28

8.1-

>58.

1 LC

M

SD

QQ

Q

ESI

+ YE

S YE

S 0.

01

NO

A

gile

nt 6

410B

10

A

CN

D

SPE

C18

2

Both

18

7 Ea

ch B

atc

h

040

Con

firm

ed w

ith

seco

nd m

etho

d

2 2

LC

TOF

ESI

+ N

O

NO

YES

Agi

lent

623

0 10

A

CN

N

one

Eclip

se C

18

3 A

uto

apro

x 50

0

041

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2.5%

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

0.00

5 m

g/kg

N

O

AG

ILEN

T

G-6

410A

10

A

CN

PS

A

ZORB

AX-

ECLI

PSE

XDB-

C8

20

Aut

o 14

3

042

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

2 tra

nsiti

ons

LC

MSD

Q

QQ

ES

I +

YES

YES

N

O

API

400

0 10

A

CN

Q

uEC

hERS

C

18 A

qua

10

Bo

th

046

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

LC

M

SD

QQ

Q

ESI

+ N

O

NO

W

ate

rs X

evo

10

Ace

tone

/PE/

DC

M

Na2

SO4

C18

2

Both

28

6 Ea

ch B

atc

h

047

Fully

iden

tifie

d

(SA

NC

O/1

2495

/201

1 p.

74-8

0)

0

2 tra

nsiti

ons +

io

n ra

tio

LC

MSD

Q

QQ

ES

I +

YES

YES

5-10

00

µg/k

g N

O

Wa

ters

Qua

ttro

Prem

ier X

E 15

A

ceto

ne/P

E/D

CM

N

O

Acq

uity

BEH

(1

00x2

.1 m

m i.

d.)

5 Bo

th

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ANNEX 1. List of Laboratories that participate in EUPT-FV-SM04.


COUNTRY LABORATORY NAME CITY REPORTED RESULTS

AUSTRIA AUSTRIAN AGENCY FOR HEALTH AND FOOD

SAFETY, COMPETENCE CENTER FOR RESIDUES OF PLANT PROTECTION PRODUCTS

INNSBRUCK YES

BELGIUM FYTOLAB ZWIJNAARDE YES

BELGIUM LOVAP GEEL YES

BELGIUM SCIENTIFIC INSTITUTE OF PUBLIC HEALTH BRUXELLES YES

CZECH REPUBLIC CZECH AGRICULTURE AND FOOD INSPECTION AUTHORITY PRAHA YES

CZECH REPUBLIC INSTITUTE OF CHEMICAL TECHNOLOGY PRAGUE, DEPT. OF FOOD CHEMISTRY AND ANALYSIS PRAGUE YES

DENMARK DANISH VETERINARY AND FOOD ADMINISTRATION REGION EAST RINGSTED YES

DENMARK NATIONAL FOOD INSTITUTE, TECHNICAL UNIVERSITY OF DENMARK SOEBORG YES

EGYPT CENTRAL LAB OF RESIDUE ANALYSIS OF PESTICIDES AND HEAVY METALS IN FOODS DOKKI, GIZA YES

ESTONIA LABORATORY FOR RESIDUES AND CONTAMINANTS, AGRICULTURAL RESEARCH CENTRE SAKU YES

FINLAND FINNISH CUSTOMS LABORATORY ESPOO YES

FRANCE CERECO SUD GARONS YES

FRANCE GIRPA BEAUCOUZE YES

FRANCE LABORATOIRE DU SCL DE MONTPELLIER MONTPELLIER YES

FRANCE LABORATORY SCL-RENNES RENNES YES

FRANCE SERVICE COMMUN DES LABORATOIRES - LABORATOIRE SCL D'ILE DE FRANCE MASSY CEDEX YES

GERMANY BAYERISCHES LANDESAMT FÜR GESUNDHEIT UND LEBENSMITTELSICHERHEIT ERLANGEN YES

GERMANY CHEMICAL AND VETERINARY ANALYTICAL INSTITUTE MUENSTERLAND-EMSCHER LIPPE MUENSTER YES

GERMANY EUROFINS DR. SPECHT LABORATORIEN GMBH HAMBURG YES

GERMANY FEDERAL OFFICE OF CONSUMER PROTECTION AND FOOD SAFETY (BVL) BERLIN YES

GERMANY GALAB LABORATORIES GMBH GEESTHACHT YES

GERMANY INSTITUTE FOR HYGIENE AND ENVIRONMENT HAMBURG YES

GERMANY LABOR FRIEDLE GMBH REGENSBURG YES

GERMANY LUA SACHSEN, DEUTSCHLAND DRESDEN YES

GERMANY NIEDERSAECHSISCHES LANDESAMT FUER

VERBRAUCHERSCHUTZ UND LEBENSMITTELSICHERHEIT, LVI OLDENBURG

OLDENBURG YES

GREECE PESTICIDE RESIDUES LABORATORY, D CHEMICAL

DIVISION, GENERAL CHEMICAL STATE LABORATORY

ATHENS YES

HUNGARY AGRICULTURAL OFFICE, DPPSCA PESTICIDE RESIDUE ANALYTICAL LABORATORY, MISKOLC MISKOLC YES

HUNGARY WESSLING HUNGARY LTD. FOOD TESTING LABORATORY BUDAPEST YES

IRELAND THE PESTICIDE CONTROL LABORATORY CELBRIDGE YES

ANNEX 1. List of Laboratories that participate in EUPT-FV-SM04.


COUNTRY LABORATORY NAME CITY REPORTED RESULTS

ITALY AGENZIA REGIONALE PROTEZIONE AMBIENTALE-LABORATORIO DI PORDENONE PORDENONE YES

ITALY ARPA PUGLIA DIPARTIMENTO DI BRINDISI BRINDISI NO

ITALY ARPA VENETO, S.L. VERONA VERONA YES

ITALY LABORATORIO CONTAMINANTI AMBIENTALI - ISTITUTO ZOOPROFILATTICO SPERIMENTALE

UMBRIA MARCHE PERUGIA YES

ITALY LANDESAGENTUR FÜR UMWELT - LABOR FÜR CHROMATOGRAPHIE BOZEN YES

ITALY SERVIZIO LABORATORIO CHIMICO - TOSSICOLOGICO ARPACAL COSENZA YES

LATVIA INSTITUTE OF FOOD SAFETY, ANIMAL HEALTH AND ENVIRONMENT "BIOR" RIGA YES

NORWAY

BIOFORSK - NORWEGIAN INSTITUTE FOR AGRICULTURAL AND ENVIRONMENTAL RESEARCH, PLANT HEALTH AND PLANT PROTECTION DIVISION,

PESTICIDE CHEMISTRY SECTION

AAS YES

ROMANIA LABORATORY FOR PESTICIDES RESIDUES CONTROL IN PLANTS AND VEGETABLE PRODUCTS BUCHAREST YES

ROMANIA SANITARY VETERINARY AND FOOD SAFETY DIRECTORATE BUCHAREST YES

SERBIA CENTER FOR FOOD ANALYSIS BELGRADE YES

SLOVENIA INSTITUTE OF PUBLIC HEALTH MARIBOR, ENVIRONMENTAL PROTECTION INSTITUTE MARIBOR YES

SPAIN LABORATORIO AGROALIMENTARIO DE GRANADA (ATARFE)

ATARFE (GRANADA) YES

SPAIN LABORATORIO AGROALIMENTARIO DE LA GENERALITAT VALENCIANA BURJASSOT YES

SPAIN LABORATORIO AGROALIMENTARIO Y DE SANIDAD ANIMAL

EL PALMAR (MURCIA) YES

SPAIN LABORATORIO DE SANIDAD VEGETAL OVIEDO NO

SWEDEN EUROFINS FOOD & AGRO SWEDEN AB LIDKÖPING YES

SWEDEN NATIONAL FOOD AGENCY (NFA), CHEMICAL UNIT 1 UPPSALA YES

SWITZERLAND SERVICE DE LA CONSOMMATION ET DES AFFAIRES VETERINAIRES (SCAV) GENEVE YES

THE NETHERLANDS NVWA - NETHERLANDS FOOD AND CONSUMER PRODUCT SAFETY AUTHORITY WAGENINGEN YES

THE NETHERLANDS RIKILT WAGENINGEN YES

TURKEY MSM FOOD CONTROL LABORATORY MERSIN YES

UNITED KINGDOM EUROFINS LABORATORIES LTD WOLVERHAMPTON YES

UNITED KINGDOM THE FOOD AND ENVIRONMENT RESEARCH AGENCY (FERA) YORK YES

ANNEX 2. Specific Protocol.


EUPT-FV-SM04 SPECIFIC PROTOCOL European Union Proficiency Test for

Pesticide Residues in Fruits and Vegetables

Screening Multiresidue Methods

(2012) Introduction

This protocol is complementary to the General Protocol for EU Proficiency Tests (EUPT) dealing with Pesticide Residues in Food and Feed. This

Proficiency Test is organised by the EURL for Pesticide Residues in Fruits and Vegetables and covers the screening of pesticides using multiresidue

methods of analysis.

The aim of this test is to evaluate laboratory capability when using large-scope quantitative and/or screening methods during routine analysis, for

detecting and identifying unexpected pesticides at levels at, or above 0.01 mg/kg – included in and/or in addition to the laboratories’ quantitative

methods used for frequently-detected pesticides. A second aim is to encourage official laboratories to extend the scope of their methods in a cost-

effective way, by using the different MS instruments/software and methods available (whether old or new).

Test material

This proficiency test is based on the pesticide-residue analysis of pears. The pears were grown in Aragón, Spain.

The pesticide treatments will be carried out post-harvest using either commercial formulation in micro-spray solutions or using standard solutions. The

test material will be frozen (using liquid nitrogen), chopped, homogenised and sub-sampled into polyethylene bottles that have previously been

coded.

Ten of these bottles containing the test material will be chosen randomly and analysed to check for homogeneity.

The test material will be stored frozen (–20ºC) prior to shipment to participants.

Two bottles, again chosen randomly, will be analysed over a period of time to confirm the stability of the pesticides in the test material (firstly, when

the test materials are shipped, and then a few days after the deadline for receipt of participants´ results). There will be a further analysis during this

period reproducing the sample shipment i.e. maintaining the sample at room temperature for a few days to see if there is any degradation of any

of the pesticides present in the test material.

These results will not be included in the statistical analysis of the proficiency test. The aim is solely to check pesticide stability during the shipping

process and for the duration of the proficiency test.

Steps to follow

This Proficiency Test will be made up of the following 6 essential steps:

1. To participate, each laboratory must complete the Application Form online, available on the EURL-FV Web page, before the deadline

stipulated on the Calendar.

2. Laboratories will then receive an e-mail confirming their participation in this exercise, and assigning them a unique Laboratory Code. With

this code, laboratories will be able to access the restricted area containing the reply forms using their login information - consisting of their

USER NAME, which is the Laboratory Code expressed as Labxxx (three digits with no spaces between them) and their PASSWORD, as chosen

on the application form.

3. The sample delivery will be free of charge to those laboratories already participating in EUPT-FV14. For those who are not EUPT-FV14

participants, please see Cost for shipment of the test material for further details. The payment procedure must have started before 20th

February. An e-mail showing the bank transfer confirmation, or similar, must have been sent beforehand, or may be requested by the

Organiser at any time. Payments without a Laboratory Code or Invoice Number to identify them will not be considered paid.

4. When the participant laboratories receive the test material (and not before), they must enter the restricted area and submit Form 0 - Test

Material Receipt to inform the Organiser that they have accepted the test material. If no test material has been received by 23rd February,

please contact the Organiser by e-mail ([email protected] and [email protected]).

5. The participating laboratories must respect the deadline for submitting the results. Results must be reported using Form 1 - Results within 72

hours after the arrival of the test item.

6. The Organiser will evaluate the results at the end of the proficiency test, once the deadline for the receipt of results has passed. The

Organiser will prepare a Preliminary Report that will be sent to the participants and uploaded to the website to show the pesticides reported,

ANNEX 2. Protocols.


after the revision of all the data by the Scientific Panel a Final Report will be done and the organiser will upload an electronic version on the

EURL-FV website and, afterwards, send a hard copy to each participant laboratory. This report will include information regarding the design

of the test, the homogeneity and stability test results, an evaluation of the participant’s results as well as graphical displays of the results and

any conclusions. Any other relevant information considered of value may also be included.

Amount of Test Material

Participants will receive:

• Approximately 300 g of pear test material treated with pesticides.

• Approximately 300 g of ‘blank’ pear test material.

Shipment of Test Materials

All test materials will be frozen and packed in polystyrene boxes surrounded by dry ice and packed into cardboard boxes.

The shipment of the test materials will start on 20th February 2012. An information message will be sent out by e-mail before shipment. Laboratories

must make their own arrangements for the receipt of the package. They must inform the Organiser of any public holidays in their country/city during

the delivery period given in the calendar as well as making the necessary arrangements to receive the shipment, even if the laboratory is closed.

Advice on Test Material Handling

Once received, the test material should be stored deeply frozen (-18°C or less) prior to analysis to avoid any possible deterioration/spoilage. The test

material should be mixed thoroughly before taking the analytical portion(s).

All participants should use their own routine standard operating procedures for extraction, clean-up and analytical measurement and their own

reference standards for identification.

Form 0 - Test Material Receipt

Once the laboratory has received the test material, the Organiser must be notified using Form 0 in the restricted area; filling in the date of receipt,

the condition of the test material, and acknowledging its acceptance. If the laboratory does not inform the Organiser by 23rd February 2012 (at the

latest) via email (to [email protected] and [email protected]), stating that no sample has been received, the Organiser will assume that the test material

has been received and accepted.

Form 1 - Results

Laboratories must enter their results in Form 1 by accessing the restricted area on the EURL-FV web site: http://www.eurl-pesticides.eu

On this form, the laboratory should report the name of each of the pesticides detected.

Each pesticide may be reported more than once if it has been detected by more than one method or identification criteria, as long as details of

each method used are also provided.

Information on the parameters and/or criteria used for detecting and reporting the pesticides found will be requested, such as deviation from

expected retention time, and MS identification details.

The idea is to ascertain if the methods are used in routinely or just specifically for this test and if the identification is undertaken manually or

automatically. Moreover, the range over which your method operates will be required. This is the concentration range - the minimum and

maximum level of your screening method that is used to detect pesticides.

Information in this form will be saved and may be changed or updated up to 72 hours after sample arrival in the laboratory. After the deadline,

results submission and/or changes to the results form will no longer be possible.

Calendar

ACTIVITY DATE

Publishing the Calendar and Matrix on the EURL-FV Web page. 30th November 2011

Submission of Application Form by invited laboratories. 15th Dec. 2011-18th Jan 2012

Sample distribution. 20th February 2012

Submission of sample receipt and acceptance - Form 0. As soon as sample is received

Deadline for receiving results - Form1 72 hours after receiving the sample

Preliminary Report. March 2012

Final Report distributed to the Laboratories. December 2012

ANNEX 2. Specific Protocol.


Cost for shipment of the test material

Only those laboratories not participating in EUPT-FV 14 will have to pay the following fee for sample shipment: EU and EFTA laboratories will be

charged 175€ and other laboratories will be charged 200 €. For the payment procedures, each laboratory can specify their details and requests for

invoices when applying for the test. Payment details are as follows:

BANK NAME: CAJAMAR - Caja Rural Sociedad Corporativa de Crédito

BANK ACCOUNT OWNER: Universidad de Almeria

BANK ADDRESS: Office Number 990. Universidad de Almeria. Spain

ACCOUNT NUMBER: 30580130172731005000

IBAN: ES0730580130172731005000

SWIFT: CCRIES2A

CONCEPT: Invoice No. or Lab Code

Contact information

The official organising group details are as follows:

Universidad de Almería. Edificio Químicas CITE I

Ctra. Sacramento s/n

04120 Almería - Spain

Fax No.: +34 950015483

Organising team (e-mail and phone no.):

Dr. Amadeo R. Fernández-Alba EURL-FV [email protected] +34 950015034

Dr. Paula Medina Pastor EURL-FV [email protected] +34 950015531

Ms. Carmen Ferrer Amate EURL-FV [email protected] +34 950015645

Mr. Octavio Malato Rodriguez EURL-FV [email protected] +34 950214423

Quality Control Group

Dr. Antonio Valverde, Senior Chemist, University of Almería, Spain.

Mr. Stewart Reynolds, Senior Chemist, FERA, York, United Kingdom.

Statistical Group

Dr. Carmelo Rodriguez, Senior Mathematician, University of Almeria, Spain.

Advisory Group

Dr. André de Kok, Senior Chemist, NVWA, Wageningen, The Netherlands.

Dr. Tuija Pihlström, Senior Chemist NFA, Uppsala, Sweden.

Dr. Sonja Masselter, Senior Chemist, AGES, Innsbruck, Austria.

Dr. Darinka Stajnbaher, Senior Chemist, IPH, Maribor, Slovenia.

Dr. Magnus Jezussek, Senior Chemist, LGL, Erlangen, Germany.

Dr. Miguel Gamón, Senior Chemist, Laboratorio Agroalimentario, Valencia, Spain.

Dr. Mette Erecius Poulsen, Senior Chemist, DTU, Copenhagen, Denmark.

Mr. Ralf Lippold, Senior Chemist, CVUA, Freiburg, Germany.

Dr. Michelangelo Anastassiades, Senior Chemist, CVUA, Stuttgart, Germany.

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