First workshop on pesticide analysis by HC11112920163

VIEWS: 16 PAGES: 40

									                   First workshop on
                   pesticide analysis
            Isabelle Windal & Vincent Hanot




22 February 2007       1st Workshop on pesticide   1
                   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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                           NRL
                                                       NRL




               NRL
                                                             NRL


                                     CRL

                   NRL                                       NRL



                         NRL                        NRL




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                           NRL
                                                       NRL




               NRL
                                                             NRL


                                     CRL

                   NRL                                       NRL



                         NRL                        NRL




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        CRL                                                        CRL
     Cereals and                                          Fruit and Vegetables
    Feeding Stuff                                           (Almeria, Spain)
(Copenhagen, Denmark)




                             Luis Martin-Plaza
             CRL
  Single Residue Methods                                         CRL
   for Pesticide Residues                                   Food of Animal
     (Fellbach, Germany)                                and Commodities with
                                                          High Fat Content
                                                         (Freiburg, Germany)



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        CRL                                                        CRL
     Cereals and                                          Fruit and Vegetables
    Feeding Stuff                                           (Almeria, Spain)
(Copenhagen, Denmark)




                             Luis Martin-Plaza
             CRL
  Single Residue Methods                                         CRL
   for Pesticide Residues                                   Food of Animal
     (Fellbach, Germany)                                and Commodities with
                                                          High Fat Content
                                                         (Freiburg, Germany)



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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 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
22 February 2007 –               of Interest to send
                     Expression 1st Workshop on pesticide or receive trainees   9
       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 Tasks
4. Organisation of proficiency tests




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                   CRL Tasks
5. Workshops and labs training




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                   CRL Tasks

6. Guideline drafting




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                    CRL Tasks
7.    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  NRL
2. CRL Fellbach  NRL & all official labs
3. 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


22 February 2007   1st Workshop on pesticide   26
         SANCO > < 657/2002/EC
                         SANCO                   657/2002/EC

       Matrices      Key matrices                 All matrices
      Recovery
                     No (70-110%)                     Yes
      correction
                     3
   Mass id-points                                      3
                     (2 if m/z>200)
                    Inter-laboratory            Within-laboratory
     Uncertainty
                    reproducibility             reproducibility
     Standard
                            25%                    individual
     uncertainty
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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)
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,..)




22 February 2007      1st Workshop on pesticide   38
           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




22 February 2007       1st Workshop on pesticide   40

								
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