First workshop on pesticide analysis

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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 2006
• Freiburg
• Fellbach
• 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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CRL
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CRL
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CRL Cereals and Feeding Stuff (Copenhagen,
Denmark)
CRL Fruit and Vegetables (Almeria, Spain)
CRL Single Residue Methods for Pesticide
Residues (Fellbach, Germany)
CRL Food of Animal and Commodities with High
Fat Content (Freiburg, Germany)
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CRL Cereals and Feeding Stuff (Copenhagen,
Denmark)
CRL Fruit and Vegetables (Almeria, Spain)
CRL Single Residue Methods for Pesticide
Residues (Fellbach, Germany)
CRL Food of Animal and Commodities with High
Fat Content (Freiburg, Germany)
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CRL Tasks

• 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
  Representative
• Pesticides 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

1. Method development

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CRL Tasks

• 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 Tasks

1. Organisation of proficiency tests

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CRL Tasks

• Workshops and labs training

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CRL Tasks

1. Guideline drafting

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CRL Tasks

1. 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

• CRL Freiburg ? NRL
• CRL Fellbach ? NRL all official labs
• 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
• organochlorines,
• pyrethroids and
• 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
• Pesticides guidelines SANCO/10232/2006
• Pesticides in all food products
• Commission decision 2002/657/EC Organic residues
  and contaminants in meat, fish, eggs, milk and
  honey

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SANCO gt lt 657/2002/EC
SANCO 657/2002/EC
Matrices Key matrices All matrices
Recovery correction No (70-110) Yes
Mass id-points 3 (2 if m/zgt200) 3
Uncertainty Inter-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 Fellbach

• Collaboration between with three CRLs Fruit and
  Vegetables (Almeria, Spain), Cereals and Feeding
  Stuff (Copenhagen, Denmark), Single Residue
  Methods for Pesticide Residues (Fellbach,
  Germany)
• Tasks of the CRLs
• Scientific Presentation
• 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 - FV (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 FV

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1st Workshop on pesticide

• Questions, remarks,
• Thank you for your attention