sanco/2004/03401 work programmes for community...

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SANCO/2004/03401

WORK PROGRAMMES FOR

COMMUNITY REFERENCE LABORATORIES

2005 **********

VETERINARY PUBLIC HEALTH (Residues)

1. Berlin (Group of substances: A5, B2a, B2b and B2e)

2. Fougères (Group of substances: A6, B1 and B3e)

3. Bilthoven (Group of substances: A1, A2, A3, A4, B2d and B3d)

4. Rome (Group of substances: B2c, B3a, B3b and B3c)

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WORK PROGRAMME FOR THE COMMUNITY REFERENCE LABORATORY BERLIN

FOR RESIDUE TESTING, 2005

Group of substances: A5-B2a-B2b-B2e

I. LEGAL FUNCTIONS AND DUTIES

The functions and duties of the Reference Laboratory are described in Annex V of Council Directive 96/23/EC (Official Journal of the European Communities No L 125 of 23 May 1996).

1. OBJECTIVES FOR THE PERIOD JANUARY - DECEMBER 2005

1.1. General tasks (5 %)

1.2. Development and validation of analytical methods (29 %) Annex V, chapter 2, section 1 (a, c, d)

1.3. Quality assurance and quality control including the development of incurred test material and the organisation of a proficiency test (22 %) Annex V, chapter 2, section 1 (a, b, c, g)

1.4. Technical and scientific support to Member States and the Commission including arbitration and training activities (44 %) Annex V, chapter 2, section 1 (d,f,l)

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2. WORKING PLAN FOR THE PERIOD JANUARY - DECEMBER 2005

2.1. General Tasks

1. Meeting 4 CRLs; EC-4 CRL for residues management 2. EC/CRL related EC and International Bodies; Co-operation with internat. Organisat. CCRVDF, CCMAS, BIPM, JRC-IRMM

3. Reports, costs estimate, documentation

2.2. Development and Validation of Analytical Methods

1. Enlargement of method for anticoccidials by LC-MSMS to further analytes (method already existing at the CRL Berlin)

The multi-residue method for anticoccidials in liver and egg by LC-MSMS, which was developed and validated last year, shall be extended to and validated for the following analytes: Laidlomycin, Semduramycin, Toltrazuril, Toltrazurilsulfone, Toltrazurilsulfoxide, Diclazuril, Clazuril, Halofuginone, Robenidin, Amprolium, Clopidol, Decoquinate, Arprinocid, Ethopabat, .Dinitolimide, Nitromide, Tinidazole. It will then cover the following analytes: Nicarbazin (as Dinitricarbanilide), Narasin, Lasalocid, Maduramycin, Saliniomycin, Monensin, Laidlomycin, Semduramycin, Toltrazuril, Toltrazurilsulfone, Toltrazurilsulfoxide, Diclazuril, Clazuril, Halofuginone, Robenidin, Amprolium, Clopidol, Decoquinate, Arprinocid, Ethopabat, .Dinitolimide, Nitromide, Tinidazole

2. Adaptation of nitroimidazole GC-MS method to LC-MSMS

The GC-MS method with negative chemical ionisation existing at the CRL Berlin shall be adapted to the LC-MSMS technique, which is becoming more and more important, in order to be able to carry out comparative examinations on commutability and to pass on the experiences made

3. Optimisation of beta-agonist multi-residue method for urine by LC-MSMS

At first, the multi-residue method for beta-agonists in liver seemed to be applicable also to urine. However, closer examinations showed that for some analytes in urine an improvement regarding recovery and precision was necessary. Therefore the existing method shall be optimised in this respect.

4. Validation of method for beta-agonists in urine by LC-MSMS

The optimised LC-MSMS method for beta-agonists in urine shall be validated with the help of InterVal. The method covers 19 different substances as well as, in addition, some deuterated internal standards. It will be checked comprehensively, especially with regard to robustness.

5. Studies on commutability of nitroimidazole analyses regarding techniques, lyophilisation and serum-plasma

As already discovered in the framework of proficiency tests, the efficiency of a method can vary strongly depending on the way of application. For example, lyophilised material can show considerable interferences though the method applied works very stably for fresh material. In the same way, different analytical techniques can have different effects on measurement results. Studies on these questions shall be carried out at the Reference Laboratory in order to discover possible effects and to pass on the information gained. Information is also needed with regard to the application of serum instead of plasma in the control of nitroimidazoles. For these investigations incurred material shall be used and comparative examinations shall be performed.

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6. Research and identification of unknown compounds

This topic comprises the search for newly developed substances which bear the risk of misuse, as well as the determination of marker substances, e. g. metabolites. At present the focus is especially on the beta-agonist group, but also on the group of anticoccidials which have gained attention in connection with the new regulations on feed additives as well as with recent cases of contamination

2.3. Quality assurance and quality control including the development of incurred test material and the organisation of a proficiency test

1. Maintenance of equipment, documentation, audits, management

According to CR 93/99/EC and CD 98/179/EC, official laboratories have to be accredited. The maintenance of a comprehensive QA system requires extensive documentation, audit and control activities in order to be able to produce reliable, reproducible and, as far as possible, traceable results. Especially in a reference laboratory a very high level of quality assurance should be uphelt.

2. Proficiency test: production and characterisation of the material, packaging, evaluation

Due to the high relevance of this substance group as well as with respect to the perfectible results of the 2003 proficiency test, anticoccidials were chosen as topic for the 2005 proficiency test again.

3. Production of incurred sample material; two different treatments (NSAID; Nitroimidazole)

Two bovines shall be treated with substances (still to be selected) from the group of NSAIDs in order to gain muscle, liver, kidney, blood, urine and eyes as analytical matrices, which are mainly to serve as QA material. Moreover we hope to gain a first impression concerning the distribution in different matrices.

Four pigs shall be treated with selected nitroimidazoles. Up to now, exclusively turkeys have been treated at the Reference Laboratory to examine the metabolisation and residue behaviour of nitroimidazoles. As this substance group is relevant also for pigs, whose metabolism differs considerably from that of turkeys, further studies on pigs are necessary to obtain relevant recommendations regarding analysis and sampling.

3. TECHNICAL AND SCIENTIFIC SUPPORT TO MEMBER STATES AND THE COMMISSION INCLUDING ARBITRATION AND TRAINING ACTIVITIES

1. Technical, scientific support and training

A maximum of four 1- to 2-week-training courses for official laboratories from Member States and Third Countries can be carried out. These training courses are organised on request of the individual laboratories and are adapted to their respective needs.

2. Provision of standard substances incl. procuring, storage, administration, documentation, shipment etc.

3. Analysis of official samples

depending on the kind and number of samples submitted

4. Visit to NRLs

to be agreed with the Commission

5. Organisation and performance of a workshop: measurement uncertainty

The topic “measurement uncertainty” has increasingly become a subject of discussions since the publication of the ISO GUM approach and even more so since the implementation of ISO 17025 in accredited laboratories. A great variety of interpretations and of ways to calculate the measurement uncertainty exist in this field. Also internationally, different concepts are available. For these reasons it seems sensible to discuss this topic with the NRLs in the framework of a Workshop.

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In the practical part of the Workshop, the multi-method for anticoccidials in egg and liver by LC-MSMS (cf. point B1) developed at the Reference Laboratory shall be presented.

It is understood that the above-mentioned objectives are not exclusive to other work of more immediate priority which may arise during the reference period in question.

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WORK PROGRAMME FOR THE COMMUNITY REFERENCE LABORATORY

FOR RESIDUE TESTING

AFSSA FOUGERES - LERMVD

Group of substances: B1, A6, B3e

Time 1st January to 31st December 2005

LEGAL FUNCTIONS AND DUTIES


4. OBJECTIVES FOR THE PERIOD JANUARY - DECEMBER 2005

4.1. General tasks Annex V, chapter 2, section 1 (a, f, h, j, k, l)

4.2. Development and validation of analytical methods Annex V, chapter 2, section 1 (a, c, d)

4.3. Quality assurance and quality control including the organisation and implementation of proficiency tests. Annex V, chapter 2, section 1 (b, e, g)

4.4. Technical and scientific support to NRLs and third countries Annex V, chapter 2, section 1(a, b, d, e, f, h, i, j, l)

5. WORKING PLAN FOR THE PERIOD JANUARY - DECEMBER 2005

A. General Tasks Annex V, chapter 2, section 1 (a, f, h, j, k, l)

1. Meeting 4 CRLs, CRLs residues management, Annex V, chapter 2, section 1 (j)

2. Technical and scientific support to the Commission, Annex V, chapter 2, section 1 (j)

3. Compilation of annual report and cost estimate, Annex V, chapter 2, section 1(k)

4. Co-operation with international organisations, Annex V, chapter 2, section 1 (j)

5. Documentation services, inter change of information via the website, Annex V, chapter 2, section 1(f, l)

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B. Development and Validation of Analytical Methods Annex V, chapter 2, section 1 (a, c, d)

6. Development and Confirmatory method for antimicrobials in different matrices (muscle, eggs, milk).

The method, initially developed on a LC/MSMS (API 2000) for confirmatory analysis of

antimicrobials in muscle will be transferred on a LC/MSMS (API4000), adapted and validated

for the confirmatory analysis of antimicrobials in muscle, milk and eggs.

7. Validation of a screening and confirmatory method of nifursol in poultry meat by LC/MSMS.

Nifursol, compound of the nitrofuran family, a former feed additives was not authorized. During 2004, the confirmatory method for nitrofuran bound metabolites was adapted to analyse the bound metabolites of nifursol. The validation process is planned for the beginning of 2005.

8. Research on and identification of unknown compounds, Annex V, chapter 2, section 1 (a, j)

The confirmatory method for antimicrobials, covered a large number of authorized compounds

as veterinary drugs. The method is used for the research and identification of unknown

antimicrobial residue in samples send by NRLs.

9. Validation of a screening method by biospecific interaction for screening of sulphonamides in

milk.

Our work on the characterization of performance of antibodies for biospecific interaction analysis and detection of residues will continue with the class of sulphonamides

10. Comparative study of ELISA kits.

The performance of ELISA kits, proposed by manufacturers to be applied on different matrices

(eggs, fish and eventually honey) will be determined.

C. Quality Assurance and Quality Control Annex V, chapter 2, section 1 (b, e, g)

11. Maintenance of the QA/QC system to ISO 17025

Annex V, chapter 2, section 1(b)

Our accreditation is based on a French programme listing a list of methods. Our accreditation body (Cofrac) has started a programme of accreditation of the competence of laboratories. Our objectives is to obtain the recognition of our competence in the use of microbiological and immunological methods for screening of residue, as well as our competence to use LC and GC coupled with different kind of detectors including mass spectrometer to develop and validate analytical methods applied to residue in different kind of matrices. Our accreditation will also cover the capacity to organize proficiency test.

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12. Organisation of proficiency tests (characterisation of the material, packaging, evaluation, report) Annex V, chapter 2, section 1(b, e, g)

Antimicrobials in muscle

One proficiency test will be organised in 2005 to analyse the capacity of NRL to detect and confirm presence of antimicrobials in muscle without previous information of the chemical family.

Three proficiency tests for banned substances will be organised.

Carbadox-Olaquindox - Muscle Chloramphenicol – Fish Nitrofurans – Milk or Fish

13. Production of incurred sample material Annex V, chapter 2, section 1(b, e, g)

a. Antimicrobials in pig muscle.

b. Chloramphenicol in fish.

c. Nitrofurans in milk or fish

A collaboration with a laboratory equipped with animal facilities for fish treatment and tissue

samples will be planned.

d. Antimicrobials in eggs

Feasibility studies to obtain artificially incurred materials with antimicrobials, checking of homogeneity, stability and packaging will be planned.

D. Technical and Scientific Support to NRLs in the Member States, the Commission and Third Countries Annex V, chapter 2, section 1 (a, b, d, e, f, h, i, j, l)

14.. Analytical support and training Annex V, chapter 2, section 1(a, b, d, e, f, i) Participation to SARAF training courses.

Training courses for scientist from Member states and third countries, on request.

15. Missions to NRLs and diffusion of scientific information Annex V, chapter 2, section 1(a, b, d, e, f, i)

16. Provisions of standard substances including storage, administration, documentation, shipment, etc

Annex V, chapter 2, section 1(j)

17. Analysis of official samples, Annex V, chapter 2, section 1 (h)

18. Organisation of a workshop on validation of screening methods Annex V, chapter 2, section 1 (e, i)

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Screening methods are widely used by Member States for antimicrobial residue. Unfortunately, validation process of this method is limited. The workshop will allow to discuss the principle of validation, objectives and experimental plan for validation of screening methods for authorized and non authorized compounds.

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COMMUNITY REFERENCE LABORATORIES IN THE FIELD OF VETERINARY PUBLIC HEALTH WITHIN THE EUROPEAN UNION

CRL for residues RIVM-ARO at Bilthoven, NL

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Work programme

January 2005 – December 2005

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FOR RESIDUE TESTING, RIVM, Bilthoven

HORMONAL GROWTH PROMOTING COMPOUNDS, SEDATIVES AND MYCOTOXINS

January 2005 – December 2005

LEGAL FUNCTIONS AND DUTIES

The functions and duties of the Reference Laboratory are described in the Annex V of Council Directive 96/23/EC (Official Journal of the European Communities No L 125 of 23. May 1996).

1. OBJECTIVES FOR THE PERIOD JANUARY 2005 – DECEMBER 2005

A: General Tasks.

Annex V, chapter 2, section 1 (c,fh,j,k,l)

B: Development and validation analytical methods.

Annex V, chapter 2, section 1 (a,c,d)

C: Quality Assurance and Quality control including the organisation and implementation of proficiency tests.

Annex V, chapter 2, section 1 (b,e,g).

D: Technical and scientific support to NRLs and third countries

Annex V, chapter 2, section 1(c,e,f,h,i)

2. WORK PROGRAMME FOR THE PERIOD JANUARY – DECEMBER 2005

A. General Tasks (Annex V, chapter 2, section 1 (c,fh,j,k,l)

1) Meeting 4 CRLs, CRLs for residues management Annex V, chapter 2, section 1 (j).

Participation in annual co-ordination meeting and general management activities

2) Technical and scientific support to the Commission Annex V, chapter 2, section 1 (j) ).

Upon request, technical assistance will be given to the European Commission and its offices and related institutes like the Joint Research Centre (JRC), the European Food

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Safety Authority (EFSA) and the European Agency for the Evaluation of Medicinal Products (EMEA).

3) Compilation of annual report and cost-statement Annex V, chapter 2, section 1 (k).

Annual report and cost-statement will be prepared before 1 April, 2005.

4) Co-operation with international organisation Annex V, chapter 2, section 1 (j)

Specific: EC/CRL related co-operation with International Bodies (e.g. AOACi, Eurachem, Codex, CVMP, EMEA, EFSA, JRCs) on method validation, analytical methodology and performance quality criteria (communication, co-ordination, and harmonisation) Explicit co-ordination of CCRVDF - EU/EC involvement.

5) Documentation services Annex V, chapter 2, section 1 (f,i).

Specific: Developments with respect to analytical methodology and (EU) legislation are constantly monitored. In addition, information on the use of new compounds or alternative approaches to improve the growth of livestock will be collected and use as input for future studies.

As part of the CRL-documentation services, the CRL-website will be maintained and updated on a regular basis. The website plays a central role in disseminating information to NRLs, i.e. with respect to general information, reference standards and analytical methods

An evaluation will be prepared of the Annual National Plans of 2004. As reference a list of matrix/method combinations, which was prepared by our CRL recently, will be used. When necessary, specific suggestions for improvement will be included in the report. This product will be scheduled for March 2005.

B: Development and validation of analytical methodology (Annex V, Chapter 2, section 1 (a,c,d)

6) Confirmatory methods will be developed for steroids without enzymatic or chemical deconjugation steps. Methods will focus on the use of LC-MS and van be used both for the analyses of e.g. muscle or hair (esters) or urine (glucuronide/sulphate conjugates). Such methods potentially find their field of application in testing for the illegal use of natural hormones or discriminating “natural” or “exogenous” origin. Initially, the study will focus on boldenone, but other steroids will follow. LC-MS methods for steroid-conjugates have the potential of becoming a cost-effective and highly specific analytical strategy within future control programs.

7) Development and validation of analytical methods necessary for effective inspection and control. There is an increased interest for analytical methods for serum and plasma, inclusive validation of the quantification. Studies will be undertaken to further assess the possibilities of analysing such samples for exogenous compounds. Materials were obtained during the 2004 animal experiment, which included the treatment of a bovine animal with ethynylestradiol, DES and the natural steroid 17beta-oestradiol.

8) Identification of new and unknown compounds illegally used for growth promoting purposes. Annex V, chapter 2, section 1 (a,j). On the basis of sample materials received (biological samples, cocktails or animal feed) studies will be undertaken to identify

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individual compounds. When necessary, metabolism studies will be performed and evaluated. Special attention will be given to the use of e.g. pro-hormones.

Specific products scheduled:

- Publication of method validation report: analytical methods for the detection of (endogenous) hormones in serum and plasma (related to (6)).

- Publication of method validation report on analytical methods for detection, identification and quantification of Somatotropine in biological matrices (activities stated in 2004).

- Publication of progress report “analyses of conjugates” (related to (7))

PM activities within sixth framework projects, participation in BIOCOP

- Support and activities within the follow up of the workshop on “The impact of quantitative chemical analysis in the 6th Framework program” (IQAILAN-NAS project, contract 96MA-CT-2002-04043).

- Support and consultation within the RADAR project “Biosensors for endogenic growth promoters in cattle””

C: Quality Assurance and Quality Control. (Annex V, Chapter 2, section 1 (b,e,g)

9) Maintenance of in-house QA/QC activities in consequence of the ISO 17025 accreditation of all analytical work done within the CRL Annex V, chapter 2, section 1 (b).

10) Organisation of proficiency tests of DES and Ethynylestradiol in bovine urine. Annex V, chapter 2, section 1 (e and g).

Specific products scheduled:

- Publication of report “Proficiency test Trenbolone in urine”

- Publication of report “Proficiency test DES in urine”

- Publication of report study “methylboldenone and metabolites in urine”

- Evaluation report Ethynylestradiol in urine”.

11) Production of incurred sample material. Annex V, Chapter 2, section 1(b,e,g)

An animal study in preparation of future proficiency tests scheduled for summer 2005. Compounds will be selected on the basis of the - discussion on priorities for future proficiency tests – during the 2004 workshop. Patricipants expressed an interest in proficiency tests for alternative materials like kidney-fat. Based on this the feasibility of a proficiency test will be evaluated.

D: Technical and scientific support to Member States and the Commission, inclusive arbitration and training activities. Annex V, chapter 2, section 1 (a,b,d,e,f,h,i,j,l)

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12) Analytical support and training. Annex V, Chapter 2, section 1 (a,b,d,e,f,i). Analytical support, both by means of advise or training, will be given or NRLs upon their request.

13) Missions to NRLs and diffusion of scientific information Annex V, Chapter 2, section 1 (a,b,d,e,f,i). Missions will be undertaken to specific NRLs on the basis of their individual needs, e.g. in order to discuss and evaluate the results of a proficiency test. Analytical support. A visit of the NRL in Greece in tentatively scheduled.

14) Provision of standard substances including storage, administration, documentation and shipment. Annex V, Chapter 2, section 1 (j). When necessary and possible, selected compounds will be purchased or (custom) synthesised.

15) Analyses of official samples. Annex V, Chapter 2, section 1 (h). Samples submitted by EU Member states in case of dispute between Member States or in case of analytical problems within a responsible NRL will be analysed.

16) Organisation of annual workshop on residue analysis. Annex V, chapter 2, section 1 (i) The topic will be selected on the basis of a consultation of the NRLs during the 2004 workshop, but will include a discussion and demonstration of a newly developed analytical procedure for sedatives.

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Work Programme of the Community Reference Laboratory for Residues

at the Istituto Superiore di Sanità (ISS-CRL)

Viale Regina Elena 299, 00161 Rome, Italy for the period 1 January– 31 December 2005

Group of substances: B2(c), B3(a), B3(b), B3(c)

Updated version: 30.09.2004

I S S - C R L

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FOR RESIDUE TESTING

AT THE ISTITUTO SUPERIORE DI SANITA’ (ISS-CRL)

ROME

Group of substances: B2(c), B3(a), B3(b), B3(c)

Time: 1 January – 31 December 2005 LEGAL FUNCTIONS AND DUTIES


6. OBJECTIVES FOR THE PERIOD 1 JANUARY - 31 DECEMBER 2005

6.1. General tasks Annex V, chapter 2, section 1 (a, f, h, j, k, l)

6.2. Development and validation of analytical methods Annex V, chapter 2, section 1 (a, c, d)

6.3. Quality assurance and quality control including the organisation and implementation of proficiency tests. Annex V, chapter 2, section 1 (b, e, g)

.64. . Technical and scientific support to NRLs and third countries Annex V, chapter 2, section 1(a, b, d, e, f, h, i, j, l)

7. WORKING PLAN FOR THE PERIOD 1 JANUARY – 31 DECEMBER 2005

E. General Tasks Annex V, chapter 2, section 1 (a, f, h, j, k, l) (anticipated break-down of all activities: 10 %)

1. Meeting of the 4 CRLs, CRLs residues management,

Annex V, chapter 2, section 1 (j)

The ISS-CRL will participate in the coordination meeting of the CRLs for residues and prepare the relevant documents under its responsibility as necessary in order to exchange information on the activities performed in the previous contract period, to discuss their outcome, to further progress in the harmonisation of the approaches adopted to assist the National Reference Laboratories (NRLs) for residues and to optimise their interaction with the Commission services. (anticipated break-down of these activities: 1 %; anticipated duration: as requested by the meeting and the preparation of the relevant documents)

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2. Technical and scientific support to the Commission,

Annex V, chapter 2, section 1 (h, j).

The ISS-CRL will provide the Commission services with all the necessary support, in particular as regards the management of administrative duties, the coordination with the Commission services, the harmonization of approaches and performance of activities among the NRLs and the preparation of technical and financial reports. Whenever a dispute arises between two Member States (MSs) on the results of the determination of substances under its responsibility, the ISS-CRL will offer its assistance in solving the problem. (anticipated break-down of these activities: 3 %; anticipated duration: throughout the year, as necessary)

3. Compilation of annual report and cost estimate,

Annex V, chapter 2, section 1(k)

Within the prescribed deadline of 31 March of the year following the relevant contract period a full report on the activities carried out, the major results obtained and future work to be undertaken as based on the such findings, as well as on the costs associated with the above activities, will be submitted to the Commission. (anticipated break-down of these activities: 2 %; anticipated duration: maximum three months after the completion of the contract period)

4. Co-operation with international organisations,

Annex V, chapter 2, section 1 (j)

Already existing bilateral contacts with other organisations will be further developed. The ISS-CRL will primarily cooperates with the Institute for Reference Materials and Measurements of the Joint Research Centre of the European Commission (EC-JRC-IRMM) as regards the conduct of Proficiency Testing Schemes (PTSs), the preparation of working reference materials and training activities especially designed for the MSs recently admitted to the European Union. Meetings at the European Agency for the Evaluation of Medicinal Products (EMEA) and at the Organisation for Economic Cooperation and Development (OECD) are also envisaged regarding the widening of the applicability of the principles of Good Laboratory Practice (GLP) and their possible synergism with the accreditation criteria as set forth in the ISO/IEC 17025 standard. (anticipated break-down of these activities: 2 %; anticipated duration: throughout the year, as necessary)

5. Documentation services, interchange of information via the website.

Annex V, chapter 2, section 1(a, f, l) Information on consolidated and innovative analytical methods will be made available to the NRLs as necessary and assistance will be given to them insofar as their implementation is concerned. In the same context, upon request, contacts will also be developed with the NRLs designated by third countries with specific reference to the implementation of the surveillance plans. The above information will be also conveyed to the NRLs, in continuation of activities already undertaken over the past years, through updating of the Handbooks of Analytical Methods for chemical elements, carbamates, pyrethroids, organophosphorus compounds,

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organochlorine compounds, polychlorobiphenyls, polychlorodibenzo-p-dioxins and polychlorodibenzofurans. The NRLs in the MSs will be requested to submit to the ISS-CRL revised information on the analytical methods already in use as well as on new methods which meanwhile may have been adopted. Ten new countries are now part of the EU. Therefore, a survey will be carried out to gather information on their technical capabilities and scientific expertise to perform the analytical assessments of interest. Concurrently, the Handbooks will be integrated with additional pertinent analytical methods, if available. Such Handbooks will be available both in the printed and electronic version. (anticipated break-down of these activities: 2 %; anticipated duration: throughout the year, as necessary)

F. Development and Validation of Analytical Methods Annex V, chapter 2, section 1 (a, c, d) (anticipated break-down of all activities: 40 %)

6. Confirmatory methods

6.1. Annex V, chapter 2, section 1 (a, d)

For the quantification of As, Cd, Cr, Cu, Fe, Hg, Pb and Zn in cow’s milk a method will be set up covering both sample preparation (freeze-drying and chemical digestion) and instrumental determination based on two different, widely used analytical techniques, namely Atomic Absorption Spectrometry with Electrothermal Volatilization (ETA-AAS) and Atomic Emission Inductively Coupled Plasma (AES-ICP). (anticipated break-down of these activities: 10 %; %; anticipated duration: 6 months)

7. Development and validation methods

7.1. Annex V, chapter 2, section 1 (c)

Innovative analytical methods for the determination of traces of selected pyrethroids, carbamates, organochlorine compounds and organophosphorus compounds will be investigated. Gas chromatography and high performance liquid chromatography with a suitable detection system will be used as an instrumental technique and in case of inadequacy another alternative technique will be considered. The confirmatory analyses will be carried out using two columns at different polarity or a gas chromatograph equipped with a mass spectrometer. All determination will be performed taking into the account the Maximum Residue Level (MRL) of each active ingredient in the considered matrix. As regards the quantification of methyl-Hg (the most toxic chemical species of Hg), a new method will be developed for its application to tuna fish. The results of this pilot study will be evaluated in terms of a possible validation of the methods. The analytical technique used to this end will be Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in combination with an on-line separation technique (anticipated break-down of all activities: 12 %; anticipated duration: 6 months)

8. Research on and identification of unknown compounds. 8.1. Annex V, chapter 2, section 1 (a)

The environmental contamination by Depleted Uranium (DU) from a number of anthropic sources is raising more and more concern. Food of animal origin is suspected to significantly

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contribute to the overall exposure of man to this chemical substance. A preliminary study will be thus carried out to have a first estimate of the presence of the 235 and 238 isotopes of U in fish and milk. Sector Field Inductively Coupled Plasma Mass Spectrometry (SF-ICP-MS) will be the analytical technique of election given its detection power and its ability to discriminate between the different isotopes of a same chemical element. (anticipated break-down of these activities: 12 %; anticipated duration: 4 months)

G. Quality Assurance and Quality Control Annex V, chapter 2, section 1 (b, e, g)

(anticipated break-down of all activities: 40 %)

9. Maintenance of the QA/QC system to ISO/IEC 17025

Annex V, chapter 2, section 1(b)

All the activities relevant to accreditation status of the ISS-CRL according to the ISO/IEC Standard 17025 will be constantly run to assure that the quality system is under control (revision of the Quality Manual and of the Standard Operating Procedures, internal audits, recording, reporting and archiving activities, sample management and the like). (anticipated break-down of these activities: 15 %; anticipated duration: throughout the year, as necessary)

10. Organisation of proficiency tests.

Annex V, chapter 2, section 1(b, e, g) A number of PTSs will be organised and conducted. These will be designed so as to take into accounts both the needs of NRLs which have already participated in the PTSs of the ISS-CRL (the previous 15 MSs, Group 1) as well as those belonging to the new MSs (Group 2). In all cases, the test materials will be characterised in terms of fit-for-purpose homogeneity and stability, adequate packaging for shipping will be selected and full evaluation reports will be prepared after completion of the exercises for distribution to the Commission and to the NRLs. The planned PTSs are as follows: i) one PTS on the determination of chemical elements (As, Cd, Cr, Cu, Fe, Hg, Pb, Zn). It will consist of four runs: three will be based on synthetic solutions simulating fish digests, while the fourth one will be based on digested fish solution as well as on the not-digested fish freeze-dried material. This approach will allow to assess the influence of the digestion procedure on the analysis of fish samples. This PTS is the ninth in the series; ii) one PTS on the determination of organophosphorus substances (selected out of those listed in the Council Directive 86/363/EEC and subsequent modifications) in spiked beef extract solutions. A reasonable choice could be the preparation of two samples spiked with six active ingredients. The first sample could contain the compounds at the Maximum Residue Levels and the second one at higher levels. This PTS is the third in the series; iii) one PTS on PCBs, PCDDs, and PCDFs. The following specific contaminants will be considered: * six indicator PCBs: T3CB-28, T4CB-52, P5CB-101, P5CB-138, H6CB-153 and H7CB-180;

* twelve dioxin-like PCBs: T4CB-77, T4CB-81, P5CB-105, P5CB-114, P5CB-118, P5CB-123, P5CB-126, H6CB-156, H6CB-157, H6CB-167, H6CB-169 and H7CB-189;

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* seventeen 2,3,7,8-chlorosubstituted PCDDs (N = 7) and PCDFs (N = 10): 2,3,7,8-T4CDD, 1,2,3,7,8-P5CDD, 1,2,3,4,7,8-H6CDD, 1,2,3,6,7,8-H6CDD, 1,2,3,7,8,9-H6CDD, 1,2,3,4,6,7,8-H7CDD, O8CDD, 2,3,7,8-T4CDF, 1,2,3,7,8-P5CDF, 2,3,4,7,8-P5CDF, 1,2,3,4,7,8-H6CDF, 1,2,3,6,7,8-H6CDF, 1,2,3,7,8,9-H6CDF, 2,3,4,6,7,8-H6CDF, 1,2,3,4,6,7,8-H7CDF, 1,2,3,4,7,8,9-H7CDF and O8CDF.

If necessary, this PTS will be organised also in a simplified form for the MSs of new accession. This PTS is the third in the series. (anticipated break-down of these activities: 20 %; anticipated duration: throughout the year, as necessary)

11. Production of incurred sample material

Annex V, chapter 2, section 1(b, e, g)

To carry out the PTSs listed under point 10 above, the following materials will be prepared and characterised:

i) a sufficient amount of tuna fish fillets (from 2 to 4 kg) will be collected, fillets will be excised, chopped and freeze-dried. This material will be used as such and no spiking will be done for any of the chemical elements mentioned under point 10(i) above;

ii) a sufficient amount of beef meat will be collected (from 2 to 4 kg), extracted as necessary and the extracts spiked with the organophosphorus substances mentioned under point 10(ii);

iii) a sufficient amount of tuna fish fillets (from 5 to 10 kg) will be collected, homogenised and possibly freeze-dried. This material will be delivered to the NRLs for the performance of the PTS on PCBs, PCDDs and PCDFs mentioned under point 10(iii) above. (anticipated break-down of these activities: 11 %; anticipated duration: throughout the year, as necessary)

H. Technical and Scientific Support to NRLs in the Member States, the Commission and Third Countries Annex V, chapter 2, section 1 (a, b, d, e, f, h, i, j, l) (anticipated break-down of all activities: 10 %)

12. Analytical support and training.

Annex V, chapter 2, section 1(a, b, d, e, f, i)

The technical personnel of the NRLs in the MSs will be trained through their participation in proficiency tests as described in part C above. All performance problems detected by such proficiency tests will be examined with the interested parties in order to minimise their occurrence in future activities. (anticipated break-down of these activities: 2 %; anticipated duration: throughout the year, as necessary)

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13. Missions to NRLs and diffusion of scientific information.

Annex V, chapter 2, section 1(a, b, d, e, f, i)

Technical assistance will be given to the NRLs as required by circumstances, including visits to their premises, facilities and laboratories at the appropriate locations. In order to support in particular the NRLs in the new MSs, three visits are planned to Poland, Hungary and Lithuania. The outcome of the visits will be reported to the Commission and to the relevant NRL. (anticipated break-down of these activities: 1 %; anticipated duration: 0.5 months)

14. Provisions of standard substances including storage, administration, documentation,

shipment Annex V, chapter 2, section 1(j)

The current information on reference materials and certified reference materials will be made available to the NRLs with particular regard to their proper use, subsampling, storage and general management. (anticipated break-down of these activities: 1 %; anticipated duration: throughout the year, as necessary)

15. Analysis of official samples,

Annex V, chapter 2, section 1 (h)

When a dispute between two MSs arises, the ISS-CRL will perform the official analyses of the samples for which there is disagreement. (anticipated break-down of these activities: 1 %; anticipated duration: throughout the year, as necessary)

16. Organisation of workshops.

Annex V, chapter 2, section 1 (e, i) The results of the two PTSs mentioned under points 10(i) (chemical elements) and 10(ii) (organophosphorus substances) will be discussed during the relevant workshops. The benefits of a PTS are enhanced by such meetings as participants can better identify through the general debate and the exchange of views the possible sources of errors which can affect their experimental results. (anticipated break-down of these activities: 5 %)

sanco/2004/03401 work programmes for community...

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