New Trends on Pesticide Residue

Analysis in Foodstuffs and its

Managements

Canping Pan

China Agricultural University

Email: panc@cau.edu.cn
 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 Hazards
from Larry D. Sanders

• Consumer perception:
pesticides & food-borne diseases
• SCIENTIFIC FACTS BASED ON ANALYSIS (ranked
in order):
1. Food-borne diseases
2. Malnutrition
3. Environmental contaminants (lead/mercury)
4. Naturally occurring toxins
5. Pesticide residue
6. 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 foodgrains

production stood at 1,792 million tonnes
and 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
Loss of Food Grains
Pest
(%)
Weeds 28
Diseases 25
Insects 23
Storage 10
Rats 8
Others 6
From An Indian statistic
 2001-2009 Pesticide sales
Worldwide
2001-2009 sales
sales (million dollar) Change rate%

2001 25,760 -6.8

2002 25,150 -5.0
2003 26,710 -1.6
2004 30,725 4.7
2005 31,190 -2.5
2006 30,425 -6.5
2007 33,390 2.8
2008 40,475 10.2
2009 37,880 -0.4
data: Phillips McDougall
 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
residues
• establishment of the WTO on 1 January 1995
• Agreement on the Application of Sanitary and Phytosanitary
Measures (SPS)

• Codex Committee on Pesticide Residues (CCPR) is part of

the Joint FAO/WHO Food Standards Programme.
• Codex MRLs: facilitate international trade and protect the
health of consumers.

• 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:
link the MRLwith ADI/ARfD
JMPR procedure for mrl setting
Residue Data
残留数据 Market enforcement
Residue definition and ..
Metabolism study etc

Residue trials on STMR; HR MRL

GAP

Toxicological Intake assessment Intake Data

ADI; ARfD
Data毒理学数 Inter, national

Intake ≤ ADI; ARfD intake > ADI; ARfD

recommend MRL recommend MRL,

exceeding ADI or ARfD ?
 Importance of Residue Chemistry

Sample
Integrity Storage
Stability
Metabolism Sample
Integrity
Residue
Method Definitions Tolerance/
Suitability MRL
Field Trial
Method
Analytical Efficiency
Method Dietary
Assessment
Directions for
Use

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
Number of Range of
% with Tolerance,
Commodity
Detects Detected Values, ppm
Samples Detects LODs, ppm
ppm
Apple Juice 372 0 – – 0.009 - 0.020 0.5

Asparagus 108 1 0.9 0.015 0.009 4.0

Blueberries 726 79 10.9 0.0005 - 0.074 0.0003 - 0.009 3.5

Blueberries,
18 2 11.1 0.001 - 0.015 0.0003 - 0.009 3.5
Frozen
Broccoli 554 372 67.1 0.0005 - 0.021 0.0003 3.5

Celery 741 205 27.7 0.001 - 0.032 0.001 - 0.009 6.0

Grape Juice 745 0 – – 0.009 - 0.021 1.5

Green Beans 741 6 0.8 0.013 - 0.093 0.009 - 0.010 4.0

Green Onions (V-
186 1 0.5 0.002 0.001 NT
1)
Greens, Collard 240 56 23.3 0.010 - 0.41 0.009 - 0.010 3.5
US FDA -1996
US FDA , 2007
US FDA 2007 report
FDA 2007 cont. report
Type of Feed # of Samples Samples
Sampl with No Exceedi
es Pesticid ng
e Regulato
Residue ry
s Guidanc
e
% # % # %
Whole/Ground 115 99 86.1 3 2.6
Grains
Plant By-products 80 57 71.3 4 5.0
Mixed Feed Rations 59 34 57.6 0 0.0
Supplements/Misc. 19 17 89.5 0 0.0
Hay & Hay Products 13 10 76.9 0 0.0

Animal By-products 6 6 100.0 0 0.0

TOTALS 292 223 76.4 7 2.4

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
Pesticide(2) Total No. of Occurance % Range, ppm
Findings
DDT 229 25 0.0001-0.0289
Malathion 146 16 0.0004-0.054
Chlorpyrifos methyl 133 15 0.0002-0.031
Endosulfan 129 14 0.0001-0.034
Dieldrin 120 13 0.0001-0.020
Chlorpyrifos 67 7 0.0001-0.173
Chlorpropham 53 6 0.0004-1.622
Permethrin 53 6 0.0002-0.480
Quintozene 53 6 0.0001-0.007
Thiabendazole(3) 51 6 0.001-0.975
Hexachlorobenzene 36 4 0.0001-0.0009
Phenylphenol, o- 34 4 0.003-0.392
Carbaryl(4) 27 3 0.001-0.189
Lindane 25 3 0.0001-0.002
Heptachlor 23 3 0.0001-0.001
 Frequency of Occurrence of Pesticide Residues in the Total Diet
Study for Infant and Toddler Foods in FY 2007
Pesticide(2) Total No. of Occurence % Range, ppm
Findings
Thiabendazole(3) 39 18 0.001-0.314
Carbaryl 36 17 0.001-0.070
Endosulfan 24 11 0.0001-0.011
DDT 19 9 0.0001-0.002
Chlorpyrifos 18 8 0.0002-0.016
Chlorpropham 17 8 0.002-0.140
Malathion 14 7 0.0006-0.017
Phenylphenol, o- 13 6 0.005-0.058
Chlorpyrifos 12 6 0.0001-0.048
methyl
Benomyl(3) 10 5 0.010-0.029
Captan 10 5 0.012-0.153
Permethrin 9 4 0.0005-0.007
Dieldrin 8 4 0.0001-0.0007
 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
140
120 Tot al No. of
100 Sampl es
80 no det ect abl e
60 r esi dues
40 non- vi ol at i ve
20 r esi dues
0

Fr ui t / veg
poul t r y,

veget abl e,

Cooki e,
or gani c

or gani c
f r ui t

meat

j ui ce,
or gani c
 sample positive
Specific food Residues found
s results1
bifenthrin, diphenylamine,
fruit 34 6
thiabendazole, o-phenylphenol
carbaryl, o-phenylphenol,
fruit, organic 10 4
thiabendazole
meat 10 1 chlorpropham
poultry 14 0 no pesticide residues detected
poultry,
2 0 no pesticide residues detected
organic
vegetable 20 1 bifenthrin
vegetable,
10 0 no pesticide residues detected
organic
diphenylamine, thiabendazole,
Fruit/veg juice 132 10 imazalil, carbaryl, amitraz,
tebuconazole
Fruit/veg juice,
18 3 carbaryl, thiabendazole
organic
chlorpyrifos-methyl, diphenylamine,
Cookie 94 16
pirimiphos-methyl, thiabendazole
Cookie,
 Canada COMPLIANCE SUMMARY FOR
FRESH FRUIT AND VEGETABLE
COMMODITIES 2004-2005
Import monitoring (2004-2005):
139 violations among 24840 samples,
2610 positive

Domestic samples
11,050, 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.
 •Are our foods safe ?
• 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!
 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 residue
Debadatta 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
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.

58
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 second 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.

59
 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
 Resolution of obstacles to work sharing
– 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”
“industry: dossiers” VS “government:
64 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 Crops
TG 502: Metabolism in Rotational Crops
TG 503: Metabolism in Livestock
TG 504: Residues in Rotational Crops (Limited Field Studies)
TG 505: Residues in Livestock
TG 506: Stability of Pesticide Residues in Stored Commodities
TG 507: Nature of Pesticide Residues in processed Commodities -
High Temperature-Hydrolysis
TG 508: Magnitude of Pesticide Residues in Processed Commodities
TG 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
Chemical Toxicology Residue Eco- Environ- Product
Chemistry toxicology mental Fate Chemistry
Pyrasulfatole Australia Canada United United Australia
States States
Pyroxsulam United Australia Australia Canada United
States States
Chlorantra- United Australia United Ireland Canada
niliprole States Kingdom
Spirotetramat United Canada Austria Austria Canada
States
Thiencarbazone/ United United Canada United United
Cyprosulfamide Kingdom Kingdom States Kingdom
Saflufenacil Canada Canada United United United
*Australia States States States
peer reviewer
Fluopyram Germany United United Canada Germany
*Japan peer States States
reviewer
Penthiopyrad United Canada United United United
States States Kingdom Kingdom
 Results— Completed and Current
Joint 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 Grouping
Regulators: 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 （柑橘类水果）
Citrus fruits（柑橘类水果）
• FP 0009 （仁果类水果）
Pome fruits（仁果类水果）
• FS 0012 （核果）
Stone fruits（核果）
• FB 0018 （浆果和其它小水果）
Berries and other small fruits（浆果和其它小水果）
• FI 0030 Assorted tropical and sub-tropical fruits - inedible peel
• VB 0040 Brassica (cole or cabbage) vegetables, Head cabbages,
Flowerhead brassicas（（白菜类蔬菜,
白菜类蔬菜 结球甘蓝,结球甘蓝 十字花科蔬菜）
十字花科蔬菜）
• VC 0045 果类蔬菜，葫芦科)
果类蔬菜，葫芦科
Fruiting vegetables, Cucurbits(果类蔬菜，葫芦科
• VO 0050 Fruiting vegetables, other than Cucurbits
• VL 0053 （叶菜）
Leafy vegetables（叶菜）
• VP 0060 （豆类蔬菜）
Legume vegetables（豆类蔬菜）
• VD 0070 （豆类）
Pulses（豆类）
• VR 0075 （根茎类蔬菜）
Root and tuber vegetables（根茎类蔬菜）
• GC 0080 （谷物）
Cereal grains（谷物）
• TN 0085 （坚果）
Tree nuts（坚果）
•
 MRLs ON MINOR CROPS IN ACP
COUNTRIES – in collaboration with the
COLEACP-PIP
• 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.

80
 EU Import Tolerances - PROCESS

Focal point
Within EU Within
National Taskforce
country
on Horticulture

Priorities identified
** Approved ITs
Crop/pesticide

Approval process Trials sites

1ST PHASE

Submissions Data generated

EU-IT requested
 EU IMPORT TOLERANCES
Successes relevant to symposium
COMMODITIES WITH PESTICIDES WITH COLLABORATING
EU-IT IT AG-CHEM
• Beans with pods • Chlorothalonil COMPANIES
• Abamectin (Some)
• Mango
• Acetamiprid • Syngenta
• Okra • Cyromazine • Bayer
• Pineapple • Difenoconazole • Nisso
• Papaya • Thiametoxam • Dow
• Passion fruit • Methoxyfenozide • Bayer
• Myclobutanil • FMC
• Snow peas
• Spinosad • Arysta
• Yams • Tebuconazole
• Cassava • Trifloxystrobin
• Sweet potatoes • Bifenthrin
• Thiophanate methyl
• Spiromesifen 82
 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.”
•
 Goal: Find The ‚Best‘ MRL

• 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.
 0.7
Primary samples
0.6
Composite samples
Relative frequency

0.5

0.4

0.3 95% 97.5%

0.2

0.1

0
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]
 NAFATA MRL Calculator

Review/inspect field
trial data

More than 10% non- No Enter data into MRL

detects? spreadsheet

Yes
Examine probability plot and
lognormal test statistic
Enter data into MLE Copy MLE-based fill-in
spreadsheet values

Yes Data lognormal?

More than
15 samples?
Yes No No

Use minimum of
1 2 3
Use 95/99 Rule as MRL UCLmedian95th and 95/99 Use Mean+3SD as MRL
Rule as MRL
 Maximum Residue Levels
Lognormal Probability Plot

FAO Carbaryl Eggplant

1.0000

0.5000 y = 0.5944x - 2.1369

2
R = 0.7547

0.2500
Concentrations

0.1250

0.0625

0.0313
0.1 1 2 5 10 20 30 50 70 80 90 95 98 99 99.9

Percentiles
 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)
 Residue
Residue
DATA
DATA

No
n≥
n 3
?3 No MRL

Yes
0 HR No
(LOQ)

Distributional tests:
No. of medium
Values Does (any)
Yes Determine Calculate Less than
Lognormal regulatory
large distribution bestdistribution
distribution 95UCL95th & regulatory
>LOQ Normal limits?
limit?
pass the fit (bestcc)
(best cc) 99th percentile
test?
small Weibull Greater
No
No HR than
HR?

Yes

Minimum of
Calculate
Calculate 95UCL95th &
Mean
Mean ++3SD
4SD 99th percentile
& UCLMed95
Mean + MaxLOQ

Less than
regulatory
regulatory
Greater Yes Minimum of
Nonparametric
2009 Draft OECD
limits? than HR?
limit? methods Calculator
No No
version 2.5
Regulatory HR
limit
 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 calculations:
– 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 sample coefficient of variance
(CV = standard deviation / mean) used in the calculation is at least 0.5. A
correction factor for censored data (=data less than 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 residue.

• MRL= Maximum (mean + 4*standard deviation, 3*mean*CF, HR).

• Finally the calculated MRL is rounded as necessary
•
 Comparison with JMPR
decisions
1000.00

100.00
MRLs produced by draft calculator

Equality line
MRL Calc = MRL JMPR
10.00

1.00
0.01 0.1 1 10 100 1000

0.10

0.01
MRLs proposed by 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 Concern
Data 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

、40th CCPR : IAEA leading EWG

• 39、
• 41th CCPR: informative
• working group on method of analysis to
prepare 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.
 4 Conclusion and Discussions

• Email: panc@cau.edu.cn