Contents of Volume 1
Preface
List of contributors
Introduction
James N. Seiber
Introduction
Relationship of pesticide residue analysis, regulation, and risk assessment
Who does residue analysis and why
Challenges
References
Regulatory guidance and scientific consideration for residue
analytical method development and validation
Assessment of residue analytical methods for crops, food, feed, and
environmental samples: the approach of the European Union
Johannes Siebers and Ralf H¨anel
Introduction
Legal background
General
Council Directive 91/414/EEC
Legislation related to MRLs
Legislation related to residues limits for soil, water, and air
Provisions for residue analytical methods
Evaluation of the submitted methods
Institutional background
Validation parameters
Requirements for post-registration and monitoring (enforcement) methods
General requirements
Specific requirements
Requirements for data generation methods
General requirements
Specific requirements
Availability of analytical methods
Perspectives
Acknowledgement
References
v
vi
Contents of Volume 1
Regulatory considerations for residue analysis and methods on crops and food:
the approach of Japan
Kazuo Ogura, Hisayoshi Yamagishi and Shigeji Sugimoto
Background
Plant metabolism studies
Residue studies on crops
Residue analytical method
Preferred methodology for conducting supervised field trials
Field data (field report) presentation
Extrapolation among the formulation types
Residue definition
Market basket survey in Japan
Conclusion
Further reading
General approaches for residue analytical method development and validation
Thomas J. Class and Reiner Bacher
Introduction
Approaches to analytical method development
Properties of the analyte(s)
Functional groups of the analyte(s)
Properties of the sample material
Availability and practicality of analytical instrumentation
Consideration of time, throughput, ruggedness and quality
Practical examples
Extending the scope of the multi-residue method DFG S19
What can go wrong?
Beyond the limits
References
Best practices in establishing detection and quantification limits for pesticide
residues in foods
Johannes Corley
Introduction
Definitions
Methods for defining LOD and LOQ
IUPAC method
Propagation of errors method
Hubaux–Vos approach
Two-step approach (proposed by the US EPA)
RMSE method
The t
99
s
LLMV
method
Confirmation
Representative data
Conclusions
Acknowledgements
References
Contents of Volume 1
vii
The process of development and validation of animal drug residue methods for
US Food and Drug Administration regulatory use
Philip James Kijak and Valerie B. Reeves
Introduction
The method
Determinative procedures
Confirmatory procedures
Development of methods for regulatory use
Practicability of methods
Analyte selection
Specificity
Ruggedness
Stability
System suitability
Method criteria
Standards
Precision
Accuracy
Other considerations
Confirmatory procedure criteria
Standard operating procedures (SOPs)
Determinative procedure
Confirmatory procedure
Other considerations
The method trial
Second analyst/laboratory check
FDA review
Inter-laboratory method trial
Confirmatory procedure method trial
Non-NADA method trial
Evaluation of data and recommendation for use
Conclusion
References
Validation of analytical methods for post-registration control and monitoring
purposes in the European Union
Lutz Alder
Introduction
Evaluation of enforcement methods for food provided by manufacturers
The need for enforcement methods from the applicant
The problem with residue definition
Elements and format of method description
Assessment of validation results
Matrices in validation experiments
Test of multi-residue methods
Independent laboratory validation
Statement on extraction efficiency
Perspectives
viii
Contents of Volume 1
Validation of European standard (CEN) methods
Scope and format of CEN methods
CEN requirements for widely accepted multi-matrix/multi-residue methods
Requirements for (newer) methods with limited scope
Assessment and documentation of validation results
Validation of official methods of EU member states
Overview of existing method collections and validation requirements
Single-laboratory validation in the UK
Validation procedures of the Nordic countries
Validation of official methods in Germany
The problem of appropriate documentation of validation data
of multi-matrix/multi-residue methods
Summary and conclusion
References
Best practices in the generation and analysis of residues in crop,
food and feed
Conducting crop residue field trials in the USA
William W. John
Introduction
Description of the different types of field crop residue studies
EPA guidelines and requirements
Planning phase
Testing strategy
Crop and crop grouping
Site/location selection
Good Agricultural Practice (GAP) and use patterns
Test substance
Residue decline trials
Processing study requirement
Contract research organizations
Best practices in conducting field study
Protocol development
The test site
Test material
Application phase
Sampling phase
Sample storage and shipping
Sample preparation
Field QA components
Data presentation and communication
Summary
References
Contents of Volume 1
ix
Conducting crop residue field trials in Europe
Jeff Old
Introduction
General issues and considerations in conducting residue studies in Europe
Regulation guidelines
European comparable climatic zones/weather influences
Crop and grouping
Study planning phase
Study objectives
Role and responsibility of study personnel
Preparing the study plan
Product use pattern
Test site requirements, evaluation and selection
Best practices to conduct field studies
Evaluation and selection of field investigators and testing personnel
Preparation of field testing study plan
Test item (previously termed test substance)
Trial layout
Growing and maintenance of trial site crops
Calibration/servicing of application equipment
Test item application
Sampling of crops
Sample shipping and transportation
Sample storage
Record keeping
Good Laboratory Practice
Field QA audits and study involvement
Archiving
Conclusion
Further reading
Conducting crop residue field trials in Mexico and Latin America
Louis Russo
Introduction
Regulatory requirements
Planning a field residue trial in Latin America
Number and locations of trials
Personnel requirements
Protocol preparation
Test materials
Quality assurance
Budget considerations
Communications
Pre-implementation activities
Translation of critical documents
Preparation of the field notebook formats
Pre-meetings in testing regions
Implementation of testing procedures
GLP training and protocol discussion
Safety training
x
Contents of Volume 1
First application
Sampling and shipping
Food Quality Protection Act (FQPA) considerations
Reporting and closure
Abbreviations
Food processing of raw agricultural commodities for residue analysis
William J. Englar, Neal Ewing, John C. Peterson and
Cheryl M. Englar-Coulter
Overview of processing of agricultural commodities
Historical background
Basis for selecting a process method
Laboratory/pilot processing of agricultural commodities
Processing requirements of individual agricultural commodities
Pilot laboratory processing versus commercial processing
Effect of processing on pesticide residues
Good Laboratory Practice (GLP) regulations and their impact on the
small-scale processing procedures
Development and validation of SOPs
Development of processing protocol
Role of study personnel
Protocol deviations
Organization of a processing report
Raw data notebook
Summary report of processing procedures
Summary
References
Best practices in the implementation of a large-scale market basket residue
survey study
David J. Brookman, Kay K. Curry and Beth M. Polakoff
Introduction
General considerations
Case study (Organophosphates Market Basket Survey)
Development of study protocol
Definition of study objectives
Role and responsibilities of study personnel
Selection of products and of properties to be evaluated
Sample collection strategy
Analyses and data reporting
Implementation of sampling plan
Shopper selection and training
Sample collection, storage, shipment, receipt, and documentation
Analytical phase
Analytical method
Obtaining control commodities
Assignment of products to laboratories
Standardization of results reporting
Presentation and review of study findings
Contents of Volume 1
xi
Quality assurance functions
Interpretation of study findings
Procedures and best practices for conducting residue studies of animal health
drugs in food animals
David J. Smith, Guy R. Stehly and Michael P. Turberg
Introduction
Purpose of residue studies
Studies sponsored by the animal health industry
Other studies
Protocol development
Animal selection and animal receipt
Animal considerations for GLP studies
Other considerations in animal selection
Preparation of test article
Animal dosing
Oral administration
Parenteral administration
Other methods of drug administration
In-life sample collection
Facility considerations
Animal weights, feed and water intakes, and dose
Nutritional and environmental considerations
Sample collection
Residue analysis
Radiochemical analysis
Analysis of the marker residue
Quality control
Report
Conclusions
References
Sampling and analyses of foodstuffs from animal origin
Robin S. Readnour, Thomas J. Burnett, Douglas E. Kiehl
and Lisa D. Spurlock-Brouwer
Introduction
Sample collection and storage
Sampling and homogenization
Stability
Extraction and sample preparation
Extraction
Sample preparation
Separation and detection
Liquid chromatography
Liquid chromatography/mass spectrometry
Gas chromatography
Immunoassay
Data handling and presentation
Method validation
xii
Contents of Volume 1
Regulatory guidelines
Inter-laboratory/collaborative studies
Conclusion
References
Compound class
Anilides
Hiroko Kobayashi
Introduction
Residue analytical methods for plant materials
Nature of the residue
Analytical method
Residue analytical methods for soil
Nature of the residues
Analytical method
Analytical methodology for water
Nature of the residues
Analytical method
References
Chloroacetanilide herbicides
Amy Hackett, John Fuhrman and Chantel Van Bellinghan
Introduction
Analytical methodology for plant and animal products
Nature of the residue
Rationale for the presented methods
Description of methodology
Analytical methodology for water and soil
Nature of the residue
Rationale for the methods presented
Description of methodology
Analytical method for the determination of acetochlor and its metabolites
in plants and animals
Outline of method
Apparatus
Reagents
Analytical standards
Analytical procedure
Instrumentation
Calculation of residues
Evaluation
Analytical method for the determination of propachlor and its metabolites
in plants and animals
Outline of method
Apparatus
Reagents
Analytical standards
Analytical procedure
Instrumentation
Contents of Volume 1
xiii
Calculation of residues
Evaluation
Multi-residue analytical method for the determination of acetochlor, alachlor,
and metolachlor in aqueous samples
Outline of method
Apparatus
Reagents
Analytical standards
Analytical procedure
Calculation of residues
Evaluation
Multi-residue analytical method for the determination of acetochlor, alachlor,
and metolachlor soil metabolites in aqueous samples
Outline of method
Apparatus
Reagents
Analytical standards
Analytical procedures
Calculation of residues
Evaluation
Future directions for environmental monitoring
Acknowledgements
References
Dinitroaniline herbicides
Masako Ueji
Introduction
Analytical methodology for plant materials
Nature of the residues
Method principle
Analytical methodology for soil
Nature of the residues
Method principle
Analytical method for soil metabolites
Analytical methodology for water
Nature of the residues
Analytical method
References
Sulfonylurea herbicides
Charles R. Powley
Introduction
Analytical methodology
LC/MS/MS analysis
Crops, food and feed
Soil
Water
Conclusions and future directions
Acknowledgements
References
xiv
Contents of Volume 1
Triazine herbicide methodology
Robert A. Yokley
Introduction/general description
Analytical methodology for water samples
Water sample preparation
Analytical methodology for soil samples
Liquid–solid extraction
Sonication
Microwave extraction
Supercritical fluid extraction
Subcritical fluid extraction
On-line SFE
Analytical methodology for crops, food, feed, and animal tissues
Analytical methodology for biological fluids
Analytical methodology for air samples
Instrumentation
Gas chromatography
Liquid chromatography
Supercritical fluid chromatography
Electrochemical analysis
Other techniques
Future directions
References
Diphenyl ethers
Masako Ueji
Introduction
Analytical methodology for plant materials
Nature of the residues
Analytical method
Analytical methodology for soil
Nature of the residues
Analytical method
Analytical method for the metabolites of diphenyl ether herbicides in soil
Analytical methodology for water
Nature of the residues
Analytical method
References
Individual compounds
Bispyribac-sodium
Yoshihiro Saito, Mitsumasa Ikeda and Akira Yagi
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Contents of Volume 1
xv
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Carfentrazone-ethyl
Audrey Chen
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Analytical procedures for nonoil crop matrices
Sample extraction, filtration and concentration
Partition
Determination of carfentrazone-ethyl
Determination of acid metabolites
Analytical procedures for crop refined oils
Analytical procedures for animal matrices
Instrumentation
Method validation and quality control
Experimental design
Preparation of standards
Calculation
Time required for analysis
Accuracy and precision
Important points
Storage stability
Acknowledgements
Flucarbazone-sodium
Thomas J. Gould and Chung K. Lam
Introduction
Outline of method
Apparatus
Reagents and consumable supplies
Sampling and preparation
Procedure
Extraction
Cleanup/concentration
Chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of quantitation
Calculation of residues
xvi
Contents of Volume 1
Important points
References
Flumetralin
Robert A. Yokley
Introduction
Outline of methods
Apparatus
Reagents
Sample preparation
Soil
Plant materials
Instrumentation
Evaluation
Method
Recoveries, limit of detection (LOD) and limit of quantitation (LOQ)
Calculation of residues
Reference
Flumioxazin
Thomas Schreier
Introduction
Outline of method
Plant matrices
Soil
Water
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection and limit of quantitation
Calculation of residues
Important points
Isoxaflutole
Robert J. Seymour, Craig A. Smitley and Sabrina X. Zhao
Introduction
Outline of method
Reagents and standards
Equipment and supplies
Sampling and preparation
Extraction procedure
Manual procedure
Contents of Volume 1
xvii
Automated procedure using a Zymark Benchmate Workstation with
EasyFill module
Determination by LC/MS/MS
Evaluation
Performance criteria
Recoveries, limit of detection and limit of quantifiation
Calculation
Orbencarb
Mitsumasa Ikeda, Yoshihiro Saito and Akira Yagi
Introduction
Outline of method
Equipment
Reagents
Sample preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries and limits of detection
Calculation of residues
Important points
Liquid–liquid partition
Cleanup
Evaporation
Detection
Determination of Metabolite II in soil
Reference
Further reading
Prodiamine
Robert A. Yokley
Introduction
Outline of method
Apparatus
Reagents
Sample preparation
Air
Soil
Water
Instrumentation
Evaluation
Method
Recoveries, limit of detection(LOD) and limit of quantitation (LOQ)
Calculation of residues
Important point
xviii
Contents of Volume 1
Prohexadione-calcium
Akira Yagi, Mitsumasa Ikeda and Yoshihiro Saito
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Procedure
Extraction
Ion-exchange column chromatography
Methylation
Reversed-phased silica gel column chromatography cleanup
High-performance liquid chromatographic determination
Evaluation
Method
Recoveries and limits of detection
Calculation of residues
Important points
References
Pyraflufen-ethyl
Yuji Ikemoto
Introduction
Outline of method
Multi-residue analytical method
Apparatus
Reagents and supplies
Procedure
Total toxic residue analytical method
Apparatus
Reagents and supplies
Procedure
Evaluation
Important points
References
Pyriminobac-methyl
Akira Yagi, Mitsumasa Ikeda and Yoshihiro Saito
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Procedure
Extraction
Liquid–liquid partition (rice grain, rice straw and soil)
Cleanup
Gas-chromatographic determination
Contents of Volume 1
xix
Evaluation
Method
Recoveries and limit of detection
Calculation of residues
Important points
Method for extraction of pyriminobac-methyl from soil
Extraction of pyriminobac-methyl from rice grain and rice straw
Cleanup
GC column
Sample storage stability
References
Pyrithiobac-sodium
Yoshihiro Saito, Mitsumasa Ikeda and Akira Yagi
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Reference
Sulfentrazone
Andrey Chen
Introduction
Method description
Method development history
Outline of method
Apparatus
Reagents
Sampling and preparation
Analytical procedures for nonoil crop matrices
Sample extraction, filtration and concentration
Second reflux (conversion of SCA to DMS and release of conjugated HMS)
and filtration
C
8
SPE cartridge
C
8
SPE cartridge/first slica gel SPE cartridge
Derivatization (silylation of 3-hydroxymethyl sulfentrazone)
Second (post-derivatization) silica gel SPE cartridge
Analytical procedures for oily crop matrices
xx
Contents of Volume 1
Analytical procedures for crop refined oils
Instrumentation
Method validation and quality control
Experimental design
Preparation of standards
Calculation
Time required for analysis
Accuracy and precision
Important points
Storage stability
Acknowledgments
Terbacil
Janine E. Rose
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Derivatization
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Reference
Thenylchlor
Hiroko Kobayashi
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Determination (rice grain, soil and water)
Evaluation
Method
Recoveries and limit of detection
Calculation of residues
Important points
References
Contents of Volume 1
xxi
Trinexapac-ethyl
Yi Lin
Introduction
Outline of methods
Trinexapac-ethyl
Trinexapac
Apparatus
Reagents
Sampling and preparation
Extraction and cleanup
Trinexapac-ethyl
Trinexapac
Determination
Evaluation
Method
Recoveries, limit of detection (LOD) and limit of quantitation (LOQ)
Calculation of residues
Acknowledgments
References
Abbreviations and acronyms
Index
Contents of Volume 2
Preface
List of contributors
Recent advances in analytical technology, immunoassay and other
nonchromatographic methods
Regulatory considerations for environmental analytical methods for
environmental fate and water quality impact assessments of agrochemicals
Michael R. Barrett and Elizabeth Behl
Introduction
Regulatory perspectives
Scientific perspectives
Risk assessment perspective
Acceptance criteria of environmental analytical methods for pesticide regulation
Method submission and evaluation criteria
Validation and availability of methods and standards
Specific method development issues
Identification of unknowns/selection of analyte(s)
Detection limits/reporting limits
Extraction efficiency/mass balance
Matrix effects
Specific environmental sample analysis issues
Identification of target population in monitoring programs
Sample collection strategy: study design
Effect of inert ingredients
Field quality control issues
Conclusions: regulatory context
References
Immunoassay, biosensors and other nonchromatographic methods
Guomin Shan, Cynthia Lipton, Shirley J. Gee and Bruce D. Hammock
Introduction
Immunoassay for pesticides
Principles of immunoassays
Immunoassay formats
Data reduction
Sample collection and preparation
Development of pesticide immunoassays
Applications
PCR for products of agricultural biotechnology
Basic principles of agricultural biotechnology
xxii
Contents of Volume 2
xxiii
Basic principles of the PCR
Basic principles of real-time PCR
Applications of PCR to agricultural biotechnology
Recent advances in nucleic acid amplification and detection
Biosensors: immunosensors
Biological transducers
Conclusion
Abbreviations
Acknowledgements
References
Immunologically based assays for pesticide/veterinary medicine residues in
animal products
Weilin L. Shelver and David J. Smith
Introduction
Immunoassays and animal production agriculture
Considerations involved in immunoassay development
Immunoassay format
End user
Assay interferences
Detection levels (sensitivity)
Target tissues
Assay validation using incurred or fortified tissues
General sample treatments for eggs, milk, and meat
Eggs
Milk
Tissues
Food-animal immunoassay applications
Agrochemical residue immunoassay applications
Detection of veterinary medicine residues
Other therapeutic agents
Other antibody-based technologies
Conclusion
Abbreviations
Acknowledgements
References
Validated immunoassay methods
James F. Brady
Introduction
Enzyme immunoassays
Choice of tube or plate format
Calculation of residues
Comparison with chromatography-based methods
Requirements for validating a residue method
Examples of validated immunoassay methods
Conclusion
References
xxiv
Contents of Volume 2
Advances in methods for pesticide residues in food
Michael F. Wilson, Stewart L. Reynolds and Richard J. Fussell
Introduction
Sample processing considerations
Extraction procedures
Cleanup procedures
Instrumental techniques for detecting, identifying and quantifying pesticide
residues in food
GC
LC
Electrophoretic techniques
Immunochemical and biosensor techniques
Future developments and trends
Silicon-based technologies
Biosensors
Imprinted polymers
Analyses of chiral pesticides
References
Overview of analytical technologies available to regulatory laboratories
for the determination of pesticide residues
Alexander J. Krynitsky and Steven J. Lehotay
Introduction
Sample preparation
Extraction
Cleanup
Analytical separations and detection
Gas chromatography/mass spectrometry (GC/MS)
HPLC/MS
Capillary electrophoresis (CE)
Conclusions
Acknowledgements
References
Best practices in the generation and analyses of residues in
environmental samples
Best practices in the analysis of residues in environmental samples:
groundwater and soil-water monitoring procedures
Leslie S. Carver and Joseph R. Chepega
Introduction
Sources for the collection of groundwater samples
Monitoring wells
Water supply wells
Other groundwater sources
Groundwater sampling procedures
Pesticides of interest
Contents of Volume 2
xxv
Sample collection techniques
Sampling of other groundwater sources
Suction lysimeter installation and sampling procedures
Preparation and installation
Lysimeter sampling
Summary
References
Preparation and instrumental analysis of agrochemical residues in water samples
William M. Leimkuehler
Introduction
Regulatory issues
Historical perspectives
Sample preparation
Instrumentation
Historical perspective
Current technology: Mass spectrometry
Selected reaction monitoring (SRM)/confirmation
Matrix effects, calibration and quantitation
Quantitation
Detection limits
Applications of LC/API-MS and LC/API-MS/MS in water sample analyses
Conclusion
References
Sampling and analysis of soil
Joseph H. Massey, Scott H. Jackson, Manasi Saha and Eberhard Zietz
Introduction
Phase I: field study design and logistics
Physicochemical properties
Use-pattern considerations
Analytical considerations
Basic experimental designs for field soil dissipation studies
Additional considerations
Phase II: field study conduct
Test site selection
Test substance application
Soil sampling techniques
Phase III: sample processing and analysis
Sample homogenization
Sample extraction
Sample cleanup
Derivatization techniques
Analytical detection and quantitation techniques
Freezer storage stability
Phase IV: reporting of results
Goodness of fit testing
Models for agrochemical dissipation in soil
DT
50
versus T
1
/2
values
xxvi
Contents of Volume 2
Determining water balance and leaching potential
Weather data requirements for water balance and mobility assessments
Summary and conclusions
Abbreviations
References
Sampling sediment and water in rice paddy fields and adjacent water bodies
Hiroki Yamamoto and Kouji Nakamura
Introduction
Rice production in paddy fields
Regulatory requirements and guidelines
Study design
Study objectives
Preparation of study protocol
Study best practices
Sediment sampling
Water sampling
Sample handling and shipment
Quality control (QC) and quality assurance (QA)
Data presentation and interpretation
Conclusion
References
Monitoring of agrochemical residues in air
James E. Woodrow, Vincent Hebert and James S. LeNoir
Introduction
Sample collection techniques
Chemical vapors
Chemicals in aerosols
Trapping efficiency
Chemical vapors
Aerosols
Field sampling procedures for airborne pesticides
Localized programs
Regional field procedures
QA/QC considerations
Summary
References
Biological sampling: determining routes of wildlife exposure to pesticides
George P. Cobb and Todd A. Anderson
Introduction
Regulatory requirements and guidelines
Historical perspectives
Study designs and best practices
Define study objectives
Preparation of study protocol
Test substances
Contents of Volume 2
xxvii
Test systems
Selection of test sites
Preparation of test sites
Application phase
Sampling
Sample handling and shipment
QA and field data requirements
Data reporting
Data presentation and interpretation
Case studies overview
Case study with Diazinon 50W
Fortress-5G case study
Conclusions and recommendations
Acknowledgments
References
Best practices in conducting dislodgeable foliar residue studies
Joseph P. McClory and D. Larry Merricks
Introduction
Regulatory requirements and experimental field design
Protocol design
Test system
Justification of test system
Materials and methods – test substance
Study locations
Plot layout
Application
Foliar sampling
Soil sampling
Sampling intervals
Dislodging residue from leaf surface
Field fortifications
Analysis
Quality assurance
Results
Recommendations
References
Best practices to conduct spray drift studies
Andrew J. Hewitt and David L. Valcore
Introduction
Study designs
Study objectives
Tracer materials
Selection of sampling locations and site preparation
Sampling devices
Field data requirements
Performance criteria
xxviii
Contents of Volume 2
Covariate study designs
Summary
References
Field methods for performing farm worker exposure and re-entry studies
Richard Honeycutt
Introduction
Current field methods for measuring mixer–loader and re-entry worker exposure
to pesticide residues
Study design and protocol preparation
Site selection
Setting up a field laboratory and auxiliary equipment
Acquiring consent from study participants
Execution of the field portion of the worker exposure/re-entry study
Observations of the volunteers during the conduct of the field study
Data collection and the use of field forms
Storage and shipping of study samples
Making sense of field data from worker exposure and re-entry studies
Organizing field data
Correcting field and analytical data
Conclusions
References
Electronic record keeping in a regulated environment
Willa Garner and Carolyn Mentzer
Introduction
Management and integration of electronic records and documents
Electronic reporting requirements
Electronic data management of protocols and SOPs
Management of field data and information
Management of laboratory data and information
Selection of a data system
System qualification
Access control
Metrology
Building blocks of a metrology program
Quality assurance (QA) and data audit
Critical areas to consider for auditing field studies
Critical areas to consider for auditing analytical laboratory studies
Validation of computerized systems
System life cycle
Validation of chromatography software
Validation priority setting and risk assessment
Organizational considerations
Validation of in-house and vendor-supplied systems
Electronic archiving
Managing durability
Managing usability
Contents of Volume 2
xxix
Open and closed systems
Electronic records and electronic signatures
Storage media issues
Audit trail
Considerations for electronic submission
Creation of PDF documents
Benefits of PDF documents
Supplemental files
Central Data Exchange (CDX)
An industry perspective
Evaluator needs
United States EDS process
EPA Office of Enforcement (OE) perspective
Regulatory enforcement of electronic data management
Harmonization
Canada
European Union
References
Compound class
Alkylenebis(dithiocarbamates)
Mihai Cicotti
Introduction
Method overview
Sample preparation
Analytical method for the determination of alkylenebis(dithiocarbamates) in plant
commodities by hot acid decomposition and spectrophotometric determination
Principle of the method
Apparatus
Reagents
Solutions
Standards and standard solutions
Reflux procedure
Photometric measurement
Recovery experiments
Limit of quantitation
Methyl xanthate spectrophotometric method
Analytical method for the determination of alkylenebis(dithiocarbamates) in plant
commodities by headspace GC and flame photometric (FPD) detection
Principle of the method
Apparatus
Reagents
Solutions
Standards and standard solutions
Headspace procedure
Gas-chromatographic conditions
Recovery experiments
Conclusions
References
xxx
Contents of Volume 2
Multi-residue methods (S19) to measure azole fungicides in crop samples
Guenther Kempe
Introduction
Introduction to the method
General overview of the various modules
Identification and confirmation
Calculation
Extraction
Module E1: extraction and subsequent liquid/liquid partition for materials with
a water content exceeding 70 g/100 g and a fat content below 2.5 g/100 g
Module E2: extraction and subsequent liquid/liquid partition for materials with
a water content below 70 g/100 g and a fat content below 2.5 g/100 g
Module E3: extraction and subsequent liquid/liquid partition for materials with
a water content exceeding 70 g/100 g, a fat content below 2.5 g/100 g and a high
acid content (highly recommended for determining acid-sensitive analytes)
Module E4: two-stage extraction and liquid/liquid partition for materials with
a water content exceeding 70 g/100 g and a fat content below 2.5 g/100 g
Module E5: two-stage extraction and liquid/liquid partition for materials with
a water content below 70 g/100 g and a fat content below 2.5 g/100 g
Module GPC: gel permeation chromatography
Module C1: column chromatography on a small silica gel column
Gas chromatography with ECD and NPD
Procedure
Summary
References
Neonicotinoids
Hiroko Kobayashi
Introduction
Analytical methodology for plant materials
Nature of the residue
Analytical method principle
Analytical methodology for soil
Nature of soil residues
Analytical method
Analytical methodology for water
Nature of the residues
Analytical method
References
Oxime carbamates
Maria Elena Y. Cabusas
Introduction
Analytical methodology
Reversed-phase HPLC/fluorescence analysis
Reversed-phase HPLC/MS and HPLC/MS/MS analysis
Crops, food, feed, and animal tissue
Soil
Water
Contents of Volume 2
xxxi
Conclusions and future directions
Acknowledgements
References
Individual compounds
Azoxystrobin
Neil J. Robinson
Introduction
Outline of methodology
Crop samples
Soil
Water
Animal matrices
Air
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Sample cleanup procedures
Determination
Evaluation
Method
Recoveries, limit of detection and limit of quantification
Calculation of residues
Important points
Reference
Famoxadone
Kathryn M. Jernberg
Introduction
Outline of method
Apparatus
Plants
Soil and water
Reagents
Plants
Soil and water
Sampling and preparation
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection, and limit of quantification
Calculation of residues
Important points
xxxii
Contents of Volume 2
Fluthiacet-methyl
Mitsumasa Ikeda, Yoshihiro Saito and Akira Yagi
Introduction
Outline of method
Equipment
Reagents
Sample preparation
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries and limit of detection
Calculation of residues
Important points
Flutolanil
Yuji Ikemoto
Introduction
Outline of method
Multi-residue analytical method (for potatoes)
Apparatus
Reagents and supplies
Procedure
Evaluation
Total toxic residue analytical method (for rice plant)
Apparatus
Reagents and supplies
Procedure
Evaluation
Important points
GC/FTD method
Apparatus
Reagents and supplies
Procedure
Evaluation
GC/MS method
Apparatus
Reagents and supplies
Procedure
Evaluation
References
Hymexazol
Shingo Sadakane, Takeshi Saito, Mariko Sabi and Takeo Otsuka
Introduction
Outline of method
Contents of Volume 2
xxxiii
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Liquid–liquid partition
Determination by gas chromatography
Evaluation
Method
Limit of detection
Method recovery in plant
Important points
Imibenconazole
Fujio Ishijima
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important point
Mepanipyrim
Mitsumasa Ikeda, Yoshihiro Saito and Akira Yagi
Introduction
Outline of method
Equipment
Reagents
Sample preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries and limit of detection
Calculation of residues
Important points
Analysis of plant metabolites
Extraction rate from soil
Further reading
xxxiv
Contents of Volume 2
Mepronil
Yoshihiro Saito, Mitsumasa Ikeda and Akira Yagi
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Tebuconazole
Greg C. Mattern, Chung V. Lam and Timothy J. Grace
Introduction
Outline of method
Apparatus
Reagents/supplies and reference standards
Reagents/supplies
Reference materials
Sampling and preparation
Procedures
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limits of detection, and limits of quantification
Calculation of residues
Reference
Acetamiprid
Shigeji Sugimoto
Introduction
Outline of method
Plant
Soil
Apparatus
Reagents
Sampling and preparation
Green tea
Fruits and vegetables
Procedure
Extraction
Contents of Volume 2
xxxv
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Further reading
Alanycarb
Katsura Yagi and Noriharu Umetsu
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Saponification
Determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
Azinphos-methyl
Sean M. Moore
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction of plant material
Determination
Evaluation
Response factor
Recoveries, limit of detection and limit of quantification
Calculation of residues
Important points
Benfuracarb
Katsura Yagi and Noriharu Umetsu
Introduction
Outline of method
Apparatus
xxxvi
Contents of Volume 2
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
References
Buprofezin
Yuji Ikemoto
Introduction
Outline of method
Multi-residue analytical method (for plants)
Apparatus
Reagents and supplies
Procedure
Evaluation
Important points
GC/MS method (for plants)
Apparatus
Reagents and supplies
Procedure
Evaluation
Multi-residue analytical method (for soil)
Apparatus
Reagents and supplies
Procedure
Evaluation
GC/MS method (for water)
Apparatus
Reagents and supplies
Procedure
Evaluation
References
Cyfluthrin
Chung V. Lam and Sean M. Moore
Introduction
Outline of method
Apparatus
Reagents/supplies and reference standards
Reagents/supplies
Reference materials
Sampling and preparation
Contents of Volume 2
xxxvii
Procedures
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limits of detections, and limits of quantitation
Calculation of residues
Fenothiocarb
Akira Yagi, Mitsumasa Ikeda and Yoshihiro Saito
Introduction
Outline of method
Apparatus
Reagents
Sampling and sample preparation
Procedure
Extraction
Cleanup
Gas-chromatographic determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important points
References
Fenoxycarb
Robert A. Yokley
Introduction
Outline of methods
Apparatus
Air
Water
Soil
Pasture grass hay, forage, cucurbits, citrus, pome fruit, tree nuts,
fruiting vegetables, and cotton substrates
Animal tissues, milk, blood, and eggs
Reagents
Sample preparation
Air
Water
Soil
Plant material
Animal material
Instrumentation
Evaluation
Method
xxxviii
Contents of Volume 2
Recoveries, limit of detection (LOD) and limit of quantitation (LOQ)
Calculation of residues
Reference
Fenpyroximate
Yuji Ikemoto
Introduction
Outline of method
Multi-residue analytical method (for plants and soil)
Apparatus
Reagents and supplies
Procedure
Evaluation
Multi-residue analytical method (for water)
Apparatus
Reagents and supplies
Procedure
Evaluation
References
Hexythiazox
Shigeji Sugimoto
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Green tea
Fruits and vegetables
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Recoveries, limit of detection and limit of determination
Calculation of residues
Important point
Reference
Imidacloprid
William M. Leimkuehler and Kimberly S. Billesbach
Introduction
Outline of method
Reagents and standards
Native standards
Internal standards
Native stock solutions
Contents of Volume 2
xxxix
Mixed standard solution
Internal standard stock solutions
Mixed internal standard solution
Apparatus
Sampling and preparation
Procedure
Sample setup
Determination
Evaluation
Method
Recoveries, limit of detection (LOD) and limit of quantitation (LOQ)
Calculations
Important points
Reference
Isoxathion
Shingo Sadakane, Manabu Toujigamori, Takeshi Saito
and Yasuhiro Tsujino
Introduction
Outline of method
Apparatus
Reagents
Analytical procedure
Extraction
Partition of n-hexane and aqueous solution
Partition of acetonitrile and hexane
Florisil column chromatography
Determination
Evaluation
Method
Limit of detection
Recovery rate in plants
Milbemectin
Shingo Sadakane, Takashi Ueda, Takashi Saito, Setsuko Katsurada,
Mariko Sabi and Yasuhiro Tsujino
Introduction
Outline of method
Apparatus
Reagents
Sample preparation
Procedure
Extraction
Cleanup
Conversion of M.A
3
and M.A
4
to corresponding fluorescent anhydride
derivatives
Determination by HPLC
Evaluation
Method
xl
Contents of Volume 2
Limit of detection
Recovery from plants
Recovery from soil
Important points
Pyrimidifen
Shingo Sadakane, Takashi Ueda, Takashi Saito, Setsuko Katsurada
and Mariko Sabi
Introduction
Outline of method
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction
Cleanup
Determination
Evaluation
Method
Limit of detection
Recovery
Calculation of residue
Important point
Pyriproxyfen
Charles A. Green
Introduction
Outline of method
Fruits and vegetables
Ginned cottonseed
Nutmeats
Soil
Water
Apparatus
Reagents
Sampling and preparation
Procedure
Extraction and cleanup
Determination
Evaluation
Method
Recoveries, limit of quantitation, and limit of detection
Calculation of residues
Important points
Abbreviations and acronyms
Index
Document Outline
- Front Matter
- Table of Contents
- Introduction
- Volume I
- Regulatory Guidance and Scientific Consideration for Residue Analytical Method Development and Validation
- Assessment of Residue Analytical Methods for Crops, Food, Feed, and Environmental Samples: The Approach of the European Union
- Regulatory Considerations for Residue Analysis and Methods on Crops and Food: The Approach of Japan
- General Approaches for Residue Analytical Method Development and Validation
- Best Practices in Establishing Detection and Quantification Limits for Pesticide Residues in Foods
- The Process of Development and Validation of Animal Drug Residue Methods for US Food and Drug Administration Regulatory Use
- Validation of Analytical Methods for Post-Registration Control and Monitoring Purposes in the European Union
- Best Practices in the Generation and Analysis of Residues in Crop, Food and Feed
- Conducting Crop Residue Field Trials in the USA
- Conducting Crop Residue Field Trials in Europe
- Conducting Crop Residue Field Trials in Mexico and Latin America
- Food Processing of Raw Agricultural Commodities for Residue Analysis
- Best Practices in the Implementation of a Large-Scale Market Basket Residue Survey Study
- Procedures and Best Practices for Conducting Residue Studies of Animal Health Drugs in Food Animals
- Sampling and Analyses of Foodstuffs from Animal Origin
- Compound Class
- Anilides
- Chloroacetanilide Herbicides
- Dinitroaniline Herbicides
- Sulfonylurea Herbicides
- Triazine Herbicide Methodology
- Diphenyl Ethers
- Individual Compounds
- Bispyribac-Sodium
- Carfentrazone-Ethyl
- Flucarbazone-Sodium
- Flumetralin
- Flumioxazin
- Isoxaflutole
- Orbencarb
- Prodiamine
- Prohexadione-Calcium
- Pyraflufen-Ethyl
- Pyriminobac-Methyl
- Pyrithiobac-Sodium
- Sulfentrazone
- Terbacil
- Thenylchlor
- Trinexapac-Ethyl
- Volume II
- Recent Advances in Analytical Technology, Immunoassay and Other Nonchromatographic Methods
- Regulatory Considerations for Environmental Analytical Methods for Environmental Fate and Water Quality Impact Assessments of Agrochemicals
- Immunoassay, Biosensors and Other Nonchromatographic Methods
- Immunologically Based Assays for Pesticide/Veterinary Medicine Residues in Animal Products
- Validated Immunoassay Methods
- Advances in Methods for Pesticide Residues in Food
- Overview of Analytical Technologies Available to Regulatory Laboratories for the Determination of Pesticide Residues
- Best Practices in the Generation and Analyses of Residues in Environmental Samples
- Best Practices in the Analysis of Residues in Environmental Samples: Groundwater and Soil-Water Monitoring Procedures
- Preparation and Instrumental Analysis of Agrochemical Residues in Water Samples
- Sampling and Analysis of Soil
- Sampling Sediment and Water in Rice Paddy Fields and Adjacent Water Bodies
- Monitoring of Agrochemical Residues in Air
- Biological Sampling: Determining Routes of Wildlife Exposure to Pesticides
- Best Practices in Conducting Dislodgeable Foliar Residue Studies
- Best Practices to Conduct Spray Drift Studies
- Field Methods for Performing Farm Worker Exposure and Re-Entry Studies
- Electronic Record Keeping in a Regulated Environment
- Compound Class
- Alkylenebis(Dithiocarbamates)
- Multi-Residue Methods (S19) to Measure Azole Fungicides in Crop Samples
- Neonicotinoids
- Oxime Carbamates
- Individual Compounds
- Azoxystrobin
- Famoxadone
- Fluthiacet-Methyl
- Flutolanil
- Hymexazol
- Imibenconazole
- Mepanipyrim
- Mepronil
- Tebuconazole
- Acetamiprid
- Alanycarb
- Azinphos-Methyl
- Benfuracarb
- Buprofezin
- Cyfluthrin
- Fenothiocarb
- Fenoxycarb
- Fenpyroximate
- Hexythiazox
- Imidacloprid
- Isoxathion
- Milbemectin
- Pyrimidifen
- Pyriproxyfen
- Abbreviations and Acronyms
- Index
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