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New Trends on Pesticide Residue Analysis in Foodstuffs and its Managements Canping Pan China Agricultural University Email: [email protected]
New Trends on Pesticide Residue Analysis in Foodstuffs and its
Managements
Canping Pan
China Agricultural University
Email: [email protected]
Outline
• 1 Overview of Agriculture and Chemicals Application: Food Security and Safety
• 2 MRL and Pesticide Residues in World Foodstuffs
• 3 Pesticide Residue Management and Recent Analytical Methodologies : MRL harmonization, global data review, minor crop, crop classification, representative crop, MRL calculator,uncertainty in residue analysis, method of analysis,risk analysis principles, etc
Top Food Safety Hazardsfrom Larry D. Sanders
• Consumer perception:pesticides & food-borne diseases
• SCIENTIFIC FACTS BASED ON ANALYSIS (ranked in order):1. Food-borne diseases2. Malnutrition3. Environmental contaminants (lead/mercury)4. Naturally occurring toxins5. Pesticide residue6. Deliberate food additives
Countries by USD value of their agricultural output, as of 2006.
Modern Agriculture Faces Challenges
• Challenges � Population increase� Arable Land area � Drought� Energy crisis (bio-energy produce like maize and agric
land use)
• Strategies:� Fertilizer� pesticide is essential material for agric � GMO crops and other technical� etc
World Population and Food Security
Food production must double by 2050 to meet the demand of the world’s growing population and innovative strategies are needed to help combat hunger, which already affects more than 1 billion people in the world…
2009, a panel discussion on “New cooperation for global food security”.
From FAO website
Number and percentage of World undernourished persons
• 2005-2007:848million (13%)• 2000-2002:833million (14%)• 1995-1997:788million (14%)• 1990-1992:843million (16%)• 1979-1981:945million (21%)• 1969-1971:958million (26%)
From FAO.org
World foodgrains production likely to dip by 2.5% in 2009 -10
• In 2008-09, the global foodgrainsproduction stood at 1,792 million tonnesand is likely to fall by 2.5% in 2009-10
• global consumption is forecast to rise by five million tonnes from last month to a record 1,741 MT, mainly because of increasing use of maize to produce ethanol in the US
Agrochemicals• Worldwide, about 10,000 species of insects are
important as pest, out of 750,000 identified species. • Over 50,000 species of fungi are responsible for some
1,500 plant diseases; • Over 1,800 species of weeds out of the known 30,000
cause serious economic loss. • About 15,000 species of nematodes produce more
than 1,500 serious deleterious effects on plants. • 30 household pests are worthy of attention, like files,
fleas, bedbugs, lice, cockroaches, mites, termites and moths
• Every year pests destroy food which could be food for 135 million people.
Pesticides are effective tools for Agro-producing
6Others 8Rats10Storage 23Insects 25Diseases 28Weeds
Loss of Food Grains Loss of Food Grains Loss of Food Grains Loss of Food Grains (%)(%)(%)(%)PestPestPestPest
From An Indian statistic
2001-2009 Pesticide sales Worldwide
data: Phillips McDougall
-0.437,8802009
10.240,4752008
2.833,3902007
-6.530,4252006
-2.531,1902005
4.730,7252004
-1.626,7102003
-5.025,1502002
-6.825,7602001
Change rate%sales (million dollar)
2001-2009 sales
Advantages of Pesticides
• Cost effectiveness . • Timeliness and flexibility• Quality, quantity and price of produce . • Prevention of various problems .
• Protection of pets and humans, Enviroment
Potential adverse effects of pesticides
• Risk: Residues in food, possible health effects at high residue levels
• Ground water, Air contamination• Drift of sprays and vapour• Reduction of beneficial species• Resistance development• Harm to farmer workers
Key: Proper application and good management of Pesticides
International and inter-regional Level: FAO pesticide specification, PIC, POPs, Codex MRL
National levels:� Pesticide quality control� Pesticide registration (Efficacy, Residue, Metabolism,
Toxicology, Eco-toxicology, Impurity Profile etc)� MRL setting based on risk assessment� Monitoring of market survey, Importing MRLs� Total diet study � Environment monitoring� - Training
Risk assessment for pesticide Risk assessment for pesticide residuesresidues
•• establishment of the WTO on 1 January 1995establishment of the WTO on 1 January 1995•• Agreement on the Application of Sanitary and Agreement on the Application of Sanitary and PhytosanitaryPhytosanitary
Measures (SPS)Measures (SPS)
•• Codex Committee on Pesticide Residues (CCPR) is part of Codex Committee on Pesticide Residues (CCPR) is part of the Joint FAO/WHO Food Standards the Joint FAO/WHO Food Standards ProgrammeProgramme..
•• Codex MRLs: facilitate international trade and protect the Codex MRLs: facilitate international trade and protect the health of consumers. health of consumers.
•• Measures which might affect international trade must: Measures which might affect international trade must: � not be stricter than necessary to achieve objective � not be maintained without sufficient scientific evidence � be consistent and transparent � be based on sound scientific risk assessment.
Pesticide risk assessment:Pesticide risk assessment:link the link the MRLwithMRLwith ADI/ADI/ARfDARfD
Market enforcement
JMPR procedure for mrl setting
Residue definition and ..Metabolism study etc
Residue trials on
GAP
STMR; HR MRL
ADI; ARfDIntake assessment
Inter, national
Intake ≤ ADI; ARfD intake > ADI; ARfD
recommend MRL,
exceeding ADI or ARfD ?
recommend MRL
Toxicological Data毒理学数毒理学数毒理学数毒理学数
据据据据
Residue Data残留数据残留数据残留数据残留数据
Intake Data
Importance of Residue Chemistry
Field Trial
ResidueDefinitions
Metabolism
MethodSuitability
AnalyticalMethod
MethodEfficiency
SampleIntegrity
StorageStability
Directions forUse
SampleIntegrity
Tolerance/MRL
DietaryAssessment
From Michael A. Doherty,a lecture on puzzle at residue chemistry
2 MRL and Residues in foodstuffs
• EU,(NL…) • UK• USA, FDA• Canada• China …
• Are our foods safe ?
In the EU, as from 1 September 2008 , a new legislative framework (Regulation (EC) No
396/2005 of the European Parliament and of the Council) on pesticide residues is applicable.
Others:• DG SANCO - Standing Committee on Food Chain &
Animal Health• DG SANCO - Rapid Alert System for Food and Feed
(RASFF)• DG SANCO - Environment: Endocrine Disruptors• DG SANCO - The Food and Veterinary Office (FVO)
• Regulation vs. Directive – Regulation: directly in force in member states – Directive: must be implemented in national legislation
• Scope – All food
» fresh » processed » composite
– Feed (new) – Products must be listed in Annex I – Pesticides according to 91/414
» some need no MRL -> in Annex IV
– MRL setting under Regulation 396/2005 • Data Requirements for Residue Studies • Guidance documents• Role Rapporteur Member State (RMS) • Role European Food Safety Authority (EFSA) • Role European Commission
• Role Standing Committee of the Food Chain and Animal Health (SCFCAH)
The Rapid Alert System for Food and Feed (RASFF) –an important tool in the
EU efforts to ensure food safety
• (EU-27, Commission, EFSA and Norway, Liechtenstein and Iceland)
• notifications in 2008 :
alert (528), information (1,138) and border rejection (1,377)
– Data Requirements for Residue Studies (91/414 – OECD) • Residue definition (Risk assessment and monitoring/enforcement) • Chronic and acute exposure risk assessment endpoints • Processing factors • MRL proposals
– Guidance documents • Stability of residues • Metabolism, distribution and expression of residues (plants, animals) • Residue trials (plant products, livestock feeding studies) • Processing studies, incl. distribution peel/pulp • Proposed residue definition for risk-assessment and MRL-setting • Proposed pre-harvest intervals • Estimation of exposure from diet and other sources
– Data Compiled in Dossier
– EU regulation 396/2005 gives procedure to set MRLs
• Application of authorisation in a member state• Member state:
– evaluates necessity of MRL– requires applying for MRL– notifies Commission and EFSA – evaluates application (possibly done by RMS) – reports to Commission and EFSA
• EFSA – assesses
» suitability proposed method of analysis for routine control
» anticipated LOD » risks of exceeding ADI or ARfD
– has three months
• Commission – Prepares Regulation – Decision to be made in the SCFCAH – has three months
– EU regulation: • Official control (monitoring & enforcement)
obligatory – Directly linked to official controls of food and feed
• Official control: Regulation 882/2004 – Community reference laboratories – Requires national reference laboratories
Monitoring
• 2005 for example: A total of 62,569 samples were analysed. 349 compounds analyzed
• no residues were detected in 54.3 % of the samples, while a further 41.0 % of the
samples contained residues that were below or equal to the maximum residue limits (MRL)
laid down at EU or national level. In 4.7 % of all samples, residues above the MRL (national
or EC-MRL) were found.
2009 EU monitoring plan
http://www.efsa.europa.eu/
First 2009 Pesticide Residue Figures: UK
• 392 out of 570 samples of 16 different foods tested had no detectable residues.
• 164 samples contained levels below the maximum residue level (MRL)
• 15 incidences in 14 samples (2.6%) contained residues in excess of the legal levels. We have looked carefully at the findings and concluded that in all cases the residues found were unlikely to have resulted in any health effects for consumers."
- Dr Ian Brown , Medical News Today, UK
USDA Pesticide Data Program –Imidacloprid :Anticipated Residues
LODs, ppmDetected Values, ppmDetectsSamples
3.50.009 - 0.010 0.010 - 0.4123.3 56 240 Greens, Collard
NT0.0010.002 0.5 1 186 Green Onions (V-1)
4.00.009 - 0.0100.013 - 0.093 0.86741Green Beans
1.50.009 - 0.021––0 745Grape Juice
6.00.001 - 0.0090.001 - 0.032 27.7 205 741 Celery
3.50.0003 0.0005 - 0.02167.1372554 Broccoli
3.50.0003 - 0.0090.001 - 0.01511.1 218Blueberries, Frozen
3.50.0003 - 0.0090.0005 - 0.07410.979726 Blueberries
4.00.009 0.0150.91108Asparagus
0.50.009 - 0.020––0372Apple Juice
Tolerance, ppm
Range of % with Detects
Number of Commodity
US FDA -1996
US FDA , 2007
US FDA 2007 report
FDA 2007 cont. report
2.47 76.4 223 292 TOTALS
0.00 100.0 6 6 Animal By-products
0.00 76.9 10 13 Hay & Hay Products
0.00 89.5 17 19 Supplements/Misc.
0.00 57.6 34 59 Mixed Feed Rations
5.04 71.3 57 80 Plant By-products
2.63 86.1 99 115 Whole/Ground Grains
%# %# %
Samples Exceeding Regulatory Guidance
Samples with No Pesticide Residues
# of Samples
Type of Feed
51 Domestic Surveillance and 18 Import Samples of Animal Feed
TDS by FDA
• most frequently found residues in the TDS foods other than infant and toddler foods (those found in 2% or more of the samples), the total number of findings, and the percent occurrence in the four market baskets analyzed in FY 2007 (916 total samples).
• The five most frequently observed chemicals were: DDT, malathion, chlorpyrifos-methyl, endosulfan, and dieldrin, and are the same as those observed for the past several years.
Residues find in TDS 2007
0.0001-0.0013 23 Heptachlor
0.0001-0.0023 25 Lindane
0.001-0.1893 27 Carbaryl(4)
0.003-0.3924 34 Phenylphenol, o-
0.0001-0.00094 36 Hexachlorobenzene
0.001-0.9756 51 Thiabendazole(3)
0.0001-0.0076 53 Quintozene
0.0002-0.4806 53 Permethrin
0.0004-1.6226 53 Chlorpropham
0.0001-0.1737 67 Chlorpyrifos
0.0001-0.02013 120 Dieldrin
0.0001-0.03414 129 Endosulfan
0.0002-0.03115 133 Chlorpyrifos methyl
0.0004-0.05416 146 Malathion
0.0001-0.028925 229 DDT
Range, ppmOccurance % Total No. of Findings
Pesticide(2)
Frequency of Occurrence of Pesticide Residues in the Total Diet
Study for Infant and Toddler Foods in FY 2007
0.0001-0.00074 8 Dieldrin
0.0005-0.0074 9 Permethrin
0.012-0.1535 10 Captan
0.010-0.0295 10 Benomyl(3)
0.0001-0.0486 12 Chlorpyrifos methyl
0.005-0.0586 13 Phenylphenol, o-
0.0006-0.0177 14 Malathion
0.002-0.1408 17 Chlorpropham
0.0002-0.0168 18 Chlorpyrifos
0.0001-0.0029 19 DDT
0.0001-0.01111 24 Endosulfan
0.001-0.07017 36 Carbaryl
0.001-0.31418 39 Thiabendazole(3)
Range, ppmOccurence % Total No. of Findings
Pesticide(2)
Pesticides Residues and Metals in Processed Tomato Products, Juice products
2008-2009, CANADA
• The Food Safety Action Plan (FSAP) aims to modernize and enhance Canada's food safety system.
• 297 (290 imported, 7 domestic) processed tomato products collected and analyzed in the targeted survey. The samples included 10 different types of processed tomatoes from 13 different countries. The top import countries of processed tomato products were targeted which include the United States and Italy.
Residue and metal in Juice, 2008-2009 Canada
• The majority of the samples (78.5%) were found to contain no detectable pesticide residues and all 186 samples were in compliance with Canadian pesticide MRLs.
• These results are expected for fruit juice concentrates as it is anticipated that fewer pesticides are used on fruit intended for juice. Furthermore, processing (washing, heating, etc) may also remove or deplete pesticide residues.
Residues in Canadian Baby foods
020406080
100120140
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Tot al No. ofSampl es no det ect abl er esi dues non- vi ol at i ver esi dues
Cookie,
chlorpyrifos-methyl, diphenylamine, pirimiphos-methyl, thiabendazole
1694Cookie
carbaryl, thiabendazole318Fruit/veg juice,
organic
diphenylamine, thiabendazole, imazalil, carbaryl, amitraz, tebuconazole
10132Fruit/veg juice
no pesticide residues detected010vegetable,
organic
bifenthrin120vegetable
no pesticide residues detected02poultry,
organic
no pesticide residues detected014poultry
chlorpropham110meat
carbaryl, o-phenylphenol, thiabendazole
410fruit, organic
bifenthrin, diphenylamine, thiabendazole, o-phenylphenol
634fruit
Residues foundpositive results 1
samples
Specific food
Canada COMPLIANCE SUMMARY FOR FRESH FRUIT AND VEGETABLE
COMMODITIES 2004-2005
Import monitoring (2004-2005):
139 violations among 24840 samples, 2610 positive
Domestic samples11,050, positive:1,051, violation: 26
-Canadian Food Inspection Agency
Pesticide in Canadian processed tomato products
• The samples analysed in this targeted survey illustrated a 100% compliance rate with Canadian pesticide MRLs in processed tomato products.
• This is similar to the compliance rates seen in most fresh and processed tomato products sampled under the regular monitoring program.
• MRL set according to residue data at critical GAP (Max application rate, timing of application, maximum number of application, mininum spray interval, short PHI ) and dietary risk assessment
• GAP: efficacy, low pressure for environment and beneficial organisms
• Market survey, enforcement of MRLs; TDS study, Environmental monitoring
MRL: regulation of violation GAP, facilitate trading , safe for consumer
ADI/ARfD are reference endpoints for human, MRL level residue are of no health concern for consumer!
•Are our foods safe ?
3 Pesticide Residue Management and Recent Analytical Methodologies
-MRL harmonization efforts- Revision on Principle of risk analysis- Work sharing, global data review, - OECD residue group and FAO manual on
pesticide residue data submission- minor crop, crop classification, representative crop, - MRL calculator,- uncertainty in residue analysis, method of analysis,-others etc
3.1 MRL harmonization • Different GAPs• Crop group disharmony• Residue definition• Mrl recommendation method • Policy and Consumer’s evaluation
MRLs are not a level for identifying safe, different risk assessment -different MRLs
• Developed countries set more restricted MRLs • Importing MRLs• growing popularity of organic foods and the use of private standards
by food retailers. • scientific advice developed in an open transparent manner
Trade Barriers among Countries
EU rejects Basmati shipments over pesticide residueDebadatta Das, June 29, 2010
In a blow to India's rice exports, Basmati, world's most famous rice, is now under the European Union's scanner.
The EU claims that there is too much of the pesticide soprothiolane in the shipments.
CCPR 42th meeting and a Pre-symposium on minor crop/minor use
• Xi’an China，2010,April
Definition of residue: Factors to consider
• Composition and levels found in metabolism studies (>10%)
• Toxicological properties
• Magnitude of the Residue
• Metabolites/degradates common to other pesticides or natural compounds?
• Availability of methods (economic methods)• Have other authorities established a definition?
• No single approach applies to all situations – must be case by case.
• Guidance document: Definition of Residue (series on Testing and Assessment, No.63)
MRL harmonization : A Pilot project
In this Pilot project, CCPR will develop a process for new chemicals that allows establishment of Codex MRLs (or at least allows JMPR recommendation of Codex MRLs) before national governments establish MRLs.
• 42th CCPR:JMPR would conduct an independent, parallel review along with a global joint review team and recommend MRLs before national governments or other regional registration authorities establish MRLs on sulfoxaflor in 2011.
From Dr Brindle, BASF
58
FAO manual on data requirements of pesticide residues for the
estimation of MRLs
Brief introduction of update FAO Manual on pesticide residues• The first version of this manual, published in 1997, presented the
principles applied by the JMPR from 1963-1997
• The first official edition (2002) of the manual was published in 2002, which incorporated additional information from the JMPR reports of 1997–2001, in particular long-term dietary risk assessment placed formally in 1998 and the methods for short-term risk assessment developed in 1999,
• The second edition (2009) describes the basic principles currently applied by the FAO Panel in the evaluation of pesticide residues for recommending MRLs. Some elements of the OECD documents have been incorporated in the Manual. GLs and Guidance documents have been listed under references.
59
FAO manual on data requirements of pesticide residues for the
estimation of MRLs
Contents of the update FAO Manual: 9 Chapters,13 Appendix and 1 index
In addition to general updating of the text, the se cond edition contains new information on:
• Metabolism studies;• Requirements regarding on environmental fate;• Performance characteristics of analytical methods;• Planning and implementing supervised residue trials;• Use of residue monitoring data for estimation of maximum residue
levels for spices;• Statistical evaluation of residue data;• Calculation of burden in animals, based on expanded feed
consumption tables;• Estimation of dietary intake of residues.
3.2 Revision on Principle of risk analysis
• 41st CCPR Session it established an Electronic Working Group led by Argentina to revise the Risk Analysis Principles Applied by the Committee on Pesticide Residues
• if the periodic evaluation (15 years) abolished and the CXLs maintained,
• complexity of the issues - to retain the periodic re-evaluation procedure and
revocation of MRLs without a scientific basis?. - use conditions of the compounds may change with time,
older existing Codex MRLs may not reflect current use patterns (GAPs) and that some of the old toxicological studies and residue trials may not meet contemporary standards?.
Priority Lists of Pesticides Tables
• Naming of manufacturers in the list of priorities
• identification of the manufacturers improved transparency and significantly facilitated communication
• CCPR Committee agreed to include the names of manufactures in the Priority List of Chemicals Scheduled for Evaluation and Re-Evaluation by JMPR.
3.3 OECD Pesticides Programme:Structure
Helps OECD governments to co-operate in assessing and reducing the risks of agricultural pesticides
-harmonizing policies-providing tools
What is work sharing?• All types of sharing of work in pesticide review, from the ad-hoc
exchange of existing reviews and other information, to well structured divisions of work such as parallel reviews and joint reviews.
Beneficial: • Quality of decisions and public confidence enhanced• Scarce resources released for more refined assessment -> sounder
scientific conclusions• Review time for new and existing registrations reduced –> reduction
in backlog• Reduced uncertainty for industry• Potential for broader labels and harmonisation of MRLs (via Codex)• Benefits for addressing minor use issues
64
– Publications « Overview of Country and Regional Review Procedures for Agricultural Pesticides and Relevant Documents » & « Frequently Asked Questions about Work Sharing on Pesticide Registration Reviews »
– Future Guidance on planning joint reviews
– Harmonisation of reporting formats: dossiers, mongraphs and templates
• Templates:– are tools for electronic data submission – are formats for reporting test study summaries – are not data entry screens
OECD is developing electronic “export formats”
Resolution of obstacles to work sharing
““ industry: dossiersindustry: dossiers”” VS VS ““ government: monographsgovernment: monographs””
Sharing of national review reports and joint reviews
• Resolution of obstacles to work sharing
• Harmonization of data requirements, test guidelines and hazard/risk assessment procedures– Inventory and harmonization of data
requirements for registration (chemical pesticides and bio-pesticides)
– OECD Test Guidelines and Guidance Documents (e.g. on Pesticide Residue Chemistry)
OECD Residue Chemistry activities:Outputs
• Establishment of the Residue Chemistry Expert Group (2003)• 9 Test Guidelines
– TG 501: Metabolism in CropsTG 502: Metabolism in Rotational CropsTG 503: Metabolism in LivestockTG 504: Residues in Rotational Crops (Limited Field Studies)TG 505: Residues in LivestockTG 506: Stability of Pesticide Residues in Stored CommoditiesTG 507: Nature of Pesticide Residues in processed Commodities -
High Temperature-HydrolysisTG 508: Magnitude of Pesticide Residues in Processed CommoditiesTG 509: Crop Field Trial
• 4 Guidance Documents– Definition of Residue– Overview of Residue Chemistry Studies – Magnitude of Pesticide Residues in Processed Commodities– Pesticide Residue Analytical Methods
3.4 Goals of Joint Review Process for New Pesticide Active
Ingredients• Harmonize endpoints (ADIs; ecotox
concerns) and MRLs to the greatest extent possible.
• Maximizing resources• Broad scientific expertise and peer review
• Global market access for reduced risk pesticides
Definitions
• Joint Review: Several authorities evaluate a pesticide active ingredient at the same time-- they receive the same submission at the same time, develop a joint schedule, and divide the work; at the conclusion each makes its own independent regulatory decision with the goal (but not requirement) of harmonization of endpoint selection and MRL establishment.
• Work Sharing: One authority has completed work on a chemical and other authorities subsequently use the completed reviews in completing their own reviews on their own schedule.
Roles in a Joint Review• Roles Countries/Regional Authorities Can
Perform in a Joint Review– Primary Review: Conduct initial review of assigned
studies and write draft study evaluations; address peer review comments and write final study evaluations
– Peer Review: Conduct secondary review of assigned studies and provide comments to the primary reviewer; excellent for capacity building
– Observer: Access to all data and information; full participant in meetings and full understanding of reviews; no work assignments; excellent for capacity building
• Different countries play different roles at different times and for different chemicals
Examples of Work Splits on Recent Joint Reviews
United Kingdom
United Kingdom
United States
CanadaUnited States
Penthiopyrad
GermanyCanadaUnited States
United States
GermanyFluopyram*Japan peer reviewer
United States
United States
United States
CanadaCanadaSaflufenacil*Australia peer reviewer
United Kingdom
United States
CanadaUnited Kingdom
United Kingdom
Thiencarbazone/Cyprosulfamid e
CanadaAustriaAustriaCanadaUnited States
Spirotetramat
CanadaIrelandUnited Kingdom
AustraliaUnited States
Chlorantra-niliprole
United States
CanadaAustraliaAustraliaUnited States
Pyroxsulam
AustraliaUnited States
United States
CanadaAustraliaPyrasulfatole
Product Chemistry
Environ-mental Fate
Eco-toxicology
Residue Chemistry
ToxicologyChemical
Results — Completed and CurrentJoint Reviews (At Least Trilateral )
• PROGRESS TO DATE:– Completed: 6– In Progress: 6– 2010-2012: 9 (planned submissions)
• POWER OF “Global” PROCESS– Chlorantraniliprole : Australia, Canada, Ireland,
United Kingdom, U.S., New Zealand.– Submitted 2007– Registered in joint review countries 2008– Currently Registered in at least 36 countries and
has Codex MRLs established 2009
Global Joint Reviews Summary• Global Joint Reviews are fast becoming the
standard way of doing business• Harmonization issues still challenging
• Many advantages are evident
• All authorities are invited and welcomed to participate (in whatever capacity they desire)
• Important to ensure that International Standard Setting Bodies are not “left behind”
3.5 Minor crop/specialty crop/minor use
• Registration based on benefits• Responsibilities of registrant products
• -2007 12， Rome， Global Minor Crop Summit
Crop GroupingRegulators: accelerate MRLs system, Less redundant data to review
Industry: More crops with fewer trials
Minor Crop Farmers: Pest-management tools, Reduced trade barriers
------------------------------------------------------------------------------Possible challenges:
• Crop grouping internationally
• Efficacy tests,
• Extrapolation risk and Restrictions (use pattern, representative crop residue)
• Risk cup capacity VS analytical method, resistance, drift
Minor Crops
• minor crops: minor uses, specialty crops• Definition needed-EU Regulation 1107/2009-41th CCPR
• Guidance and Principles on the Selection of Representative Commodities for the Extrapolation of MRLs to Commodity Groups
• revision of the Classification of Foods and Feeds with the inclusion of minor crops
EWG Tasks on minor crops
• to continue to identify priority minor uses and specialty crops for MRL setting,
• and to facilitate data submissions to JMPR,
• and to prepare proposals for definitions of minor use and specialty crops for use by CCPR and JMPR.
Example： Pome fruits MRL• Summary of residue data selected for STMR,
HR and maximum residue level estimation (rank order, median underlined):
• Apples: 0.049, 0.058, 0.15, 0.16, 0.17, 0.18, 0.18, 0.19, 0.20, 0.22, 0.37, 0.38, 0.58 mg/kg.
• Pears: 0.094, 0.097, 0.10, 0.14, 0.24, 0.13 0.16, 0.29 mg/kg
• Pome fruits: 0.049, 0.058, 0.094, 0.097, 0.10, 0.13, 0.14, 0.15, 0.16, 0.16, 0.17, 0.18, 0.18, 0.19, 0.20, 0.22, 0.24, 0.29, 0.37, 0.38, 0.58 mg/kg
CAC数据库
Residue Extrapolation• FC 0001 Citrus fruits （柑橘类水果）（柑橘类水果）（柑橘类水果）（柑橘类水果）• FP 0009 Pome fruits （仁果类水果）（仁果类水果）（仁果类水果）（仁果类水果）• FS 0012 Stone fruits （核果）（核果）（核果）（核果）• FB 0018 Berries and other small fruits （浆果和其它小水果）（浆果和其它小水果）（浆果和其它小水果）（浆果和其它小水果）• FI 0030 Assorted tropical and sub-tropical fruits - i nedible peel• VB 0040 Brassica (cole or cabbage) vegetables, Head c abbages,
Flowerhead brassicas （（（（白菜类蔬菜白菜类蔬菜白菜类蔬菜白菜类蔬菜, 结球甘蓝结球甘蓝结球甘蓝结球甘蓝, 十字花科蔬菜十字花科蔬菜十字花科蔬菜十字花科蔬菜））））• VC 0045 Fruiting vegetables, Cucurbits( 果类蔬菜，葫芦科果类蔬菜，葫芦科果类蔬菜，葫芦科果类蔬菜，葫芦科)• VO 0050 Fruiting vegetables, other than Cucurbits• VL 0053 Leafy vegetables （叶菜）（叶菜）（叶菜）（叶菜）• VP 0060 Legume vegetables （豆类蔬菜）（豆类蔬菜）（豆类蔬菜）（豆类蔬菜）• VD 0070 Pulses （豆类）（豆类）（豆类）（豆类）• VR 0075 Root and tuber vegetables （根茎类蔬菜）（根茎类蔬菜）（根茎类蔬菜）（根茎类蔬菜）• GC 0080 Cereal grains （谷物）（谷物）（谷物）（谷物）• TN 0085 Tree nuts （坚果）（坚果）（坚果）（坚果）•
80
MRLs ON MINOR CROPS IN ACP MRLs ON MINOR CROPS IN ACP COUNTRIES COUNTRIES –– in collaboration with the in collaboration with the
COLEACPCOLEACP --PIPPIP• Pesticide Initiative Program (PIP):
Cooperation program between the EU and the ACP countries under the umbrella of the COLEACP.
• Developed at the request of the ACP/EU Council of Ministers at Cotonou in April 2000 the PIP to provide a response to the critical situation growers are facing as a consequence of
– the European review for the re-registration of existing substances and
– the harmonisation of the European regulations setting Maximum Residue Levels (MRL) for pesticides in fresh produce.
EU Import Tolerances - PROCESS
1ST PHASE
Data generated
Priorities identifiedCrop/pesticide
Submissions
Trials sitesApproval process
EU-IT requested
** Approved ITs
Focal pointNational Taskforce
on Horticulture
Within EU Within country
EU IMPORT TOLERANCESEU IMPORT TOLERANCESSuccesses relevant to symposiumSuccesses relevant to symposium
PESTICIDES WITH PESTICIDES WITH ITIT
• Chlorothalonil
• Abamectin• Acetamiprid
• Cyromazine
• Difenoconazole• Thiametoxam
• Methoxyfenozide
• Myclobutanil• Spinosad
• Tebuconazole
• Trifloxystrobin• Bifenthrin
• Thiophanate methyl
• Spiromesifen 82
COMMODITIES WITH COMMODITIES WITH EUEU--ITIT
• Beans with pods• Mango• Okra• Pineapple• Papaya• Passion fruit• Snow peas• Yams• Cassava• Sweet potatoes
COLLABORATING COLLABORATING AGAG--CHEM CHEM COMPANIES COMPANIES (Some)(Some)
• Syngenta
• Bayer• Nisso
• Dow
• Bayer• FMC
• Arysta
3.6 MRL calculator: transparency and precise science in mrl recommendation
• 2009, NAFTA calculator method was evaluated, (2004 -
• Review on OECD MRL calculator
• JMPR 2009 report: “…. evaluation of residue data is a complex task that requires the consideration of factors and parameters additional to the numerical residue values. Consequently, MRL estimates cannot be based solely on automatic calculation using any currently available “statistical” methods.”
•
• Statistical goal of the OECD MRL calculator:
• to produce an MRL proposal in the region of the 95th percentile (‘p95’) of the underlying residue distribution, which is conservative in the sense that it will tend ‘to make errors’ by overestimating the p95 rather than by underestimating it for most datasets.
Goal: Find The ‚Best‘ MRL
0
0.1
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0.7
0.0 0.5 0.9 1.4 1.8 2.3 2.7 3.2 3.6 4.1 4.5
Midpoint [mg/kg]
Rel
ativ
e fre
quen
cyPrimary samples
Composite samples
95% 97.5%
NAFATA MRL Calculator
Examine probability plot and lognormal test statistic
Review/inspect field trial data
More than 10% non-detects?
Enter data into MLE spreadsheet
Enter data into MRL spreadsheet
Data lognormal?
More than
15 samples?
Use Mean+3SD as MRLUse 95/99 Rule as MRLUse minimum of
UCLmedian95th and 95/99 Rule as MRL
Yes
No
No
NoYes
Yes
Copy MLE-based fill-in values
321
Lognormal Probability Plot
99.9999895908070503020105210.1
1.0000
0.5000
0.2500
0.1250
0.0625
0.03130.03130.03130.03130.03130.03130.03130.03130.03130.03130.0313
y = 0.5944x - 2.1369
R2 = 0.7547
Percentiles
Concentrations
FAO Carbaryl Eggplant
Maximum Residue Levels
General guiding principles of OECD MRL calculator project
• The procedure must be a practical implementation of sound statistical methods.
• It must be simple to use without requiring extensive statistical knowledge on the part of the user.
• It should produce a clear and unambiguous MRL proposal for most residue datasets produced by field trials.
• It should harmonize existing procedures in OECD member countries as much as possible and provide a basis to to foster MRL harmonization for interested parties (CCPR, JMPR, EFSA)
test?pass the fit
Does (any)distribution
n
Yes
No MRL
ResidueDATA
ResidueDATA
?3n ≥≥≥≥3No
0 HR(LOQ)
distribution(best cc)
Determinebest distribution
(best cc)
No
Calculate95UCL95th &
99th percentile
regulatorylimits?
Less thanregulatory
limit?
Distributional tests:
Lognormal
Normal
Weibull
No. ofValues >LOQ
regulatorylimits?
Less thanregulatory
limit?
No
No
Yes
Regulatorylimit
medium
large
small
CalculateMean + 3SD & UCLMed95
Minimum of95UCL95th &
99th percentile
Yes
Greater thanHR?
HRNo
Yes Minimum ofNonparametric
methods
CalculateMean + 4SD
Mean + MaxLOQ
No
Greater than HR?
HR
2009 Draft OECD Calculator
version 2.5
Workflow Of The New Version Of the Calculator 2010
1. The mean and the standard deviation values of the dataset are computed:
2. The calculated MRL is the maximum taken from 3 ca lculations:– the “mean + 4 times the standard deviation” value is evaluated as the
default proposal which will be most often used;– the “the triple of the mean” value is also computed to provide a “floor” to
the calculation; that is to guarantee that the samp le coefficient of variance (CV = standard deviation / mean) used in the calcul ation is at least 0.5. A correction factor for censored data (=data less tha n LOQ) has been added. The factor depends on the the percentage of censored data in the data set.
– the HR value is also used as a “floor” to guarantee that the MRL proposal is always greater than or equal to the highest residu e.
• MRL= Maximum (mean + 4*standard deviation, 3*mean*CF, HR).• Finally the calculated MRL is rounded as necessary•
Comparison with JMPR decisions
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0.10
1.00
10.00
100.00
1000.00
0.01 0.1 1 10 100 1000
MRLs proposed by JMPR
MR
Ls p
rodu
ced
by d
raft
calc
ulat
or
Equality lineMRL Calc = MRL JMPR
The graphs shows MRLs produced by the draft calculator (Y-axis) with the MRLs proposed by JMPR experts (X-axis). Both axes are represented using a logarithmic scale. The points on the blue line correspond to datasets for which the draft calculator yields an MRL-estimate that is equal to the MRL proposed by experts. Points above (below) the line correspond to datasets for which the draft calculator yields an MRL-estimate that is higher (lower) than the MRL proposed by JMPR.
3.7 pesticides analytical methods and uncertainty
Uncertainty and MRL compliance limits
Interpretation with expanded uncertainty 2007:v1
FFP
• the evaluation of the recent EC PT schemes demonstrates that a FFP variability of 25% can be accepted as a sound representation of performance under these circumstances. As a consequence, accepting 25% variability as a standard deviation would lead to a generalized assumption of ±50% MU.
• Accepting such a generalized approximation for pesticide multi-residue analysis methods, a generalized top-down approach might result in larger MU values than such derived for each individual pesticide/commodity combination by systematic bottom-up calculations.
• However, the application of generic MU is considerably more practical and easier to obtain. Generalized values, like ±50% MU, mostly would expand safety margins around MRLs.
RECOMMENDATION / PROPOSAL
empirical top-down estimation of ±50% MU could complement a mathematically stringent bottom-up calculation model if the respective empirical quality criteria are met.
Alternatively the Horwitz formula approach of estimating concentration-dependent MU based on the evaluation of results of interlaboratory collaborative tests could be applied as well.
• It is proposed to further develop a specific guidance for the application of empirical MU concepts applicable particularly in the field of pesticide residue analysis of foodstuffs.
EWG on uncertainties of pesticide residue analysis at CCPR
• Chair and co-chair: Austria and China
• CCPR 42, CRD32;
• REQUEST FOR COMMENTS AT STEP 3 ON THE PROPOSED REVISION OF THE GUIDELINES ON THE ESTIMATION OF UNCERTAINTY OF RESULTS FOR THE DETERMINATION OF PESTICIDE RESIDUES (CAC/GL 59-2006) (ALINORM 09/32/24
Analytical Methods
Analytical Methods and Residues of ConcernData Collection
• Risk assessment residues
• Enforcement residues
Enforcement• Enforcement residues
Data collection methods are often the same as enforcement methods
• ANALYSIS OF PESTICIDE RESIDUES: RECOMMENDED METHODS
• CODEX STAN 229-1993, REV.1-2003
• 39、、、、40th CCPR : IAEA leading EWG• 41th CCPR: informative
• working group on method of analysis toprepare a discussion paper for the next session, addressing the issues raised in CX/PR 10/42/15 in relation to the status of the repository list of analytical methods
• to discuss the implications of maintaining the list as either a resource list or as preferred/obligatory methods.
