22 February 2007 1st Workshop on pesticide 1

First workshop on pesticide analysis

Isabelle Windal & Vincent Hanot

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Overview

• CRL-NRL-official labs network• CRL and NRL tasks• Questionnaires• Presentation of the discussion and

conclusions of the CRL-NRL meeting in Germany in Decembre 2006FreiburgFellbach

• PT - summary

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CRL-NRL-official labs network

The European legislation describes a concept of a network of

• Community Reference Laboratory (CRL)

• And National Refernce Laboratory (NRL)

to improve the overal quality, accuracy and comparability of the results at official control laboratories

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NRL

NRL

NRL

NRL

NRL

NRL

NRL

NRL

CRL

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CRL

NRL

NRL

NRL

NRL

NRL

NRL

NRL

NRL

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CRL Cereals and Feeding Stuff

(Copenhagen, Denmark)

CRL Single Residue Methods for Pesticide Residues

(Fellbach, Germany)

CRLFruit and Vegetables

(Almeria, Spain)

CRLFood of Animal

and Commodities with High Fat Content

(Freiburg, Germany)

Luis Martin-Plaza

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CRL Cereals and Feeding Stuff

(Copenhagen, Denmark)

CRL Single Residue Methods for Pesticide Residues

(Fellbach, Germany)

CRLFruit and Vegetables

(Almeria, Spain)

CRLFood of Animal

and Commodities with High Fat Content

(Freiburg, Germany)

Luis Martin-Plaza

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CRL Tasks

1. Information management

• setup the network

• develop websites and databases in order to• Create a Pool with analytically valuable information• Exploit synergy potentials in Information Management• Spend less time in retrieving information• Facilitate Decision-Making• Define Priorities• Allow grouping (profiling) and thus selection of RepresentativePesticides and Commodities based on sound information

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CRL Tasks (infomation: continued)

Pesticide Database:• Recovery data with different methods• Degradation behaviour of pesticides• Behaviour in Analysis (partitioning, cleanup)

Commodity Database:• Amount of co-extracted components• Behaviour in cleanup• Matrix Effects

Information about Laboratories:– Contact Information (contact persons…)– Instrumentation available– Specializations– Link to web-site & annual report– Expression of Interest to send or receive trainees

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www.Pesticides-online.com

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www.crl.cvuas.de

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CRL Tasks

2. Method development

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CRL Tasks

3. Interlaboratory method validation

– On going: Acidic pesticides in cucumber, raisin, lemon, flour (15 labs) by the modified QUECHERS method or the ChemElute method

– Future : Glyphosate in cereal

– Future : Polar compounds in fruits and vegetables

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CRL Tasks4. Organisation of proficiency tests

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CRL Tasks5. Workshops and labs training

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CRL Tasks

6. Guideline drafting

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CRL Tasks7. Providing scientific and technical assistance to the

Commission, e.g. for the establishment of co-ordinated programmes

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Set priorities !!!

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NRL Tasks

• Collaboration with CRL and official labs

• Coordination of official labs activities

• Organisation of ring test at the national level

• Technical assistance

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Questionnaires

1. CRL Freiburg NRL2. CRL Fellbach NRL & all official labs3. NRL Belgium you

Only one time!! (Set up of the network!!!) Set priorities List of the labs to be invited for the

intercomparison studies

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Please fill these questionnaires !!!!

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Meeting with CRL Freiburg (food of animal origin and comodities with high fat content)

1. Proficiency test 2006 for NRL: results

2. Proficiency test 2007 for all official labs

3. Main analytical and focus points and work programme

4. Quality management and validation

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1. Proficiency test 2006

• To all NRL (20 labs)

• Scope: organochlorines, pyrethroids and organophosphorous compounds in vegetable oil

• Conclusions: labs need to Improve the number of analyte followed (only

2 labs/20 able to analyse all compounds)Decrease the spread of the results

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2. Proficiency test 2007

• To all official labs (contribution of about 200 euros)

• Scope: same than PT 2006: organochlorines, pyrethroids and organophosphorous compounds in vegetable oil (a list of 50 pesticides is provided from which10-15 pesticides are used to spike the oil)

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3. Main analytical and focus points and work programme

• 3 groups of pesticides can be considered to be included in daily routine :

1. organochlorines, 2. pyrethroids and 3. organophosphorous

• Other groups are extremely low covered• Need for exange of information about reason

for the inclusion of certain groups in maximum levels for food of animal origin and in national residue control plan.

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4. Quality management and validation

Two legislations:

1. Pesticides guidelines SANCO/10232/2006

Pesticides in all food products

2. Commission decision 2002/657/EC Organic residues and contaminants in meat, fish, eggs, milk and honey

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SANCO > < 657/2002/EC

SANCO 657/2002/EC

Matrices Key matrices All matrices

Recovery correction

No (70-110%) Yes

Mass id-points3

(2 if m/z>200)3

UncertaintyInter-laboratory reproducibility

Within-laboratory reproducibility

Standard uncertainty

25% individual

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What to do ????

Favorite option

separation of requirements for veterinary drug residue analysis (2002/657) and for analysis of pesticides and contaminants

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Chhhhuuuutttt…..

• Separation between pesticides-contaminants and veterinary drug residues is proposed at this time via the revision of the directive 96/23/EC (NB: the 657/2002 implements the 96/23/EC)

BUT• Possibly, the revision could enter into force in

2009 MUCH LATER than the entry into force of the 657/2002 (1st September 2007)

In the meantime: we have to find another solution anyway

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• Request for extension of deadline for finalization of validation of methods according to 2002/657 (so far 1st Septembre 2007)

extension of period can be used for further harmonization.

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Meeting with CRLs FellbachCollaboration between with three CRLs: Fruit and

Vegetables (Almeria, Spain), Cereals and Feeding Stuff (Copenhagen, Denmark), Single Residue Methods for Pesticide Residues (Fellbach, Germany)

1. Tasks of the CRLs

2. Scientific Presentation

3. Training

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1. Tasks : Fruit and Vegetables

• Technical and Scientific Support to the Commission, EU Members State and Third Countries

• Development and Validation of Analytical– Updating MRMs– New procedures– New MRMs– New procedures for extraction

• EU AQC Guidelines• Proficiency Tests

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1. Tasks : Cereals and Feeding Stuff

• Technical and Scientific Support to the Commission, EU Members State.

• Interlaboratory method validation on glyphosate method

• Collection and evaluation of information to support the prioritization of method development projects

• Proficiency Test – PT C1

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1. Tasks - Single Residue Methods for Pesticide Residues

• Technical and Scientific Support to the Commission, EU Members State

• Method Development– Polar Compounds Quats, Glyphosate,

certain metabolites– Dithiocarbamates– Volatile compounds Ethyleneoxide– Compounds amenable to Multiresidue

Methods after modification

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1. Tasks - Single Residue Methods for Pesticide Residues /2

• Method Validation– Acidic Pesticides (already done)– Polar Compounds in Fruits and Vegetables

Proficiency Test

• Proficiency Test– PT SRM 1 (already done) (acidic, quats, organotin)– PT C1 -collaboration

• Information Management– Pesticides on-line,…. (in collaboration with the

other CRLs)

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2. Scientific Presentation

Available on the web site

• Pesticides on-line• Glyphosate method in HPLC-MS/MS (with

membrane suppressor)• UPLC-MS/MS• TOF

– GC-TOF and GCXGC TOF (In routine but LOQ,…)

– LC-TOF (At this moment not in routine,…)

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3. Training

• Lab presentation

• Vendor Presentation

• Quechers– Need to cryo-homogenisation– New version (other salts, pH,..)

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Profiency Tests - summary• 2006 - CRL

– CRL Freiburg: OC, OP, Pyr in oil (NRLs)– PT-SRM 1 (acidic, quats, organotin in apple juice) (NRLs)– EU PT08 (All labs)

• 2006 – NRL– OC in fat

• 2007 - CRL– CRL Freiburg: OC, OP, Pyr in oil (all officials labs)– EU PT09 - Multi - F&V (all labs)– PT – CR1 Multi and single(NRL will communicate Official labs)– OC, OP, Pyr in oil (NRL have communicated official labs)

• 2007 – NRL– OC in fat– Pesticides in F&V

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1st Workshop on pesticide

Questions, remarks,…

Thank you for your attention