Handbook of Residue Analytical Methods for Agrochemicals / Edition 1

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This two-volume handbook uniquely brings together information on the key methodologies used in the analysis of agrochemical residues and current best practices, while also giving numerous examples of how these methodologies are applied in practice to a wide range of both individual compounds, and classes of agrochemical compounds.

Volume 1 describes some of the current regulatory considerations for residue analytical methods, before going on to discuss current methods for the generation and analysis of residues in crops, food and feed. Highly practical articles then focus on the methods used for a range of individual herbicide compounds and classes of herbicide compounds.

Volume 2 presents some of the key recent advances in analytical technology in this field, before going on to discuss best practices for the generation and analysis of residues in environmental samples. Highly practical articles then focus on the methods used for a range of individual fungicide and pesticide compounds, and classes of fungicide and pesticide compounds.

  • Provides the latest information in one comprehensive source - saving time and money
  • Written by leading practioners in key industrial and government laboratories
  • Includes key recent advances in analytical technology in this field
  • Provides full-length articles, compound classes and individual compounds


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Editorial Reviews

From the Publisher
"...Providing the latest information in one comprehensive source - saving time and money - this essential reference is written by leading practitioners...." ( International Pest Control, March/April 2003)
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Product Details

  • ISBN-13: 9780471491941
  • Publisher: Wiley
  • Publication date: 4/4/2003
  • Edition number: 1
  • Pages: 1552
  • Product dimensions: 7.66 (w) x 10.12 (h) x 3.48 (d)

Table of Contents



List of Contributors.

Introduction (J. Seiber).


Assessment of Residue Analytical Methods for Crops, Food, Feed, and Environmental Samples: The Approach of the European Union (J. Siebers & R. Hänel).

Regulatory Considerations for Residue Analysis and Methods on Crops and Food: The Approach of Japan (K. Ogura, et al.).

General Approaches for Residue Analytical Method Development and Validation (T. Class & R. Bacher).

Best Practices in Establishing Detection and Quantification Limits for Pesticide Residues in Foods (J. Corley).

The Process of Development and Validation of Animal Drug Residue Methods for US Food and Drug Administration Regulatory Use (P. Kijak & V. Reeves).

Validation of Analytical Methods for Post-Registration Control and Monitoring Purposes in the European Union (L. Alder).


Conducting Crop Residue Field Tri als in the USA (W. John).

Conducting Crop Residue Field Trials in Europe (J. Old).

Conducting Crop Residue Field Trials in Mexico and Latin America (L. Russo).

Food Processing of Raw Agricultural Commodities for Residue Analysis (W. Englar, et al.).

Best Practices in the Implementation of a Large-Scale Market Basket Residue Survey Study (D. Brookman, et al.).

Procedures and Best Practices for Conducting Residue Studies of Animal Health Drugs in Food Animals (D. Smith, et al.).

Sampling and Analyses of Foodstuffs from Animal Origin (R. Readnour, et al.).


Anilides (H. Kobayashi).

Chloroacetanilide Herbicides (A. Hackett, et al.).

Dinitroaniline Herbicides (M. Ueji).

Sulfonylurea Herbicides (C. Powley).

Triazine Herbicide Methodology (R. Yokley).

Diphenyl Ethers (M. Ueji).


Bispyribac-sodium (Y. Saito, et al.).

Carfentrazone-ethyl (A. Chen).

Flucarbazone-sodium (T. Gould & C. Lam).

Flumetralin (R. Yokley).

Flumioxazin (T. Schreier).

Isoxaflutole (R. Seymour, et al.).

Orbencarb (M. Ikeda, et al.).

Prodiamine (R. Yokley).

Prohexadione-calcium (A. Yagi, et al.).

Pyraflufen-ethyl (Y. Ikemoto).

Pyriminobac-methyl (A. Yagi, et al.).

Pyrithiobac-sodium (Y. Saito, et al.).

Sulfentrazone (A. Chen).

Terbacil (J. Rose).

Thenylchlor (H. Kobayashi).

Trinexapac-ethyl (Y. Lin).

Abbreviations and Acronyms.




List of Contributors.


Regulatory Considerations for Environmental Analytical Methods for Environmental Fate and Water Quality Impact Assessments of Agrochemicals (M. Barrett & E. Behl).

Immunoassay, Biosensors and Other Nonchromatographic Methods (G. Shan, et al.).

Immunologically Based Assays for Pesticide/Veterinary Medicine Residues in Animal Products (W. Shelver & D. Smith).

Validated Immunoassay Methods (J. Brady).

Advances in Methods for Pesticide Residues in Food (M. Wilson, et al.).

Overview of Analytical Technologies Available to Regulatory Laboratories for the Determination of Pesticide Residues (A. Krynitsky & S. Lehotay).


Best Practices in the Analysis of Residues in Environmental Samples: Groundwater and Soil-water Monitoring Procedures (L. Carver & J. Chepega).

Preparation and Instrumental Analysis of Agrochemical Residues in Water Samples (W. Leimkuehler).

Sampling and Analysis of Soil (J. Massey, et al.).

Sampling Sediment and Water in Rice Paddy Fields and Adjacent Water Bodies (H. Yamamoto & K. Nakamura).

Monitoring of Agrochemical Residues in Air (J. Woodrow, et al.).

Biological Sampling: Determining Routes of Wildlife Exposure to Pesticides (G. Cobb & T. Anderson).

Best Practices in Conducting Dislodgeable Foliar Residue Studies (J. McClory & D. Merricks).

Best Practices to Conduct Spray Drift Studies (A. Hewitt & D. Valcore).

Field Methods for Performing Farm Worker Exposure and Re-entry Studies (R. Honeycutt).

Electronic Record Keeping in a Regulated Environment (W. Garner & C. Mentzer).


Alkylenebis(dithiocarbamates) (M. Cicotti).

Multi-residue Methods (S19) to Measure Azole Fungicides in Crop Samples (G. Kempe).

Neonicotinoids (H. Kobayashi).

Oxime Carbamates (M. Cabusas).


Azoxystrobin (N. Robinson).

Famoxadone (K. Jernberg).

Fluthiacet-methyl (M. Ikeda, et al.).

Flutolanil (Y. Ikemoto).

Hymexazol (S. Sadakane, et al.).

Imibenconazole (F. Ishijima).

Mepanipyrim (M. Ikeda, et al.).

Mepronil (Y. Saito, et al.).

Tebuconazole (G. Mattern, et al.).

Acetamiprid (S. Sugimoto).

Alanycarb (K. Yagi & N. Umetsu).

Azinphos-methyl (S. Moore).

Benfuracarb (K. Yagi & N. Umetsu).

Buprofezin (Y. Ikemoto).

Cyfluthrin (C. Lam & S. Moore).

Fenothiocarb (A. Yagi, et al.).

Fenoxycarb (R. Yokley).

Fenpyroximate (Y. Ikemoto).

Hexythiazox (S. Sugimoto).

Imidacloprid (W. Leimkuehler & K. Billesbach).

Isoxathion (S. Sadakane, et al.).

Milbemectin (S. Sadakane, et al.).

Pyrimidifen (S. Sadakane, et al.).

Pyriproxyfen (C. Green).

Abbreviations and Acronyms.


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First Chapter

Handbook of Residue Analytical Methods for Agrochemicals, 2 Volume Set

John Wiley & Sons

Copyright © 2003 John Wiley & Sons Ltd.
All right reserved.

ISBN: 0-471-49194-2

Chapter One

Conducting crop residue field trials in the USA

William W. John DuPont Crop Protection, Stine Haskell Research Center, Newark, DE, USA

1 Introduction

The twentieth century was a period of tremendous change in American agriculture. The development, introduction, and adoption of tractors powered by an internal combustion engine totally changed the way farmers worked, the work they had to do, the time required for them to accomplish the work, and the costs associated with farm production. Along with the introduction of mechanical power and its associated labor-saving tools came new varieties of crops which were resistant to disease, and were locally adapted to environmental conditions so that high productivity was achievable throughout the USA. The introduction of commercial fertilizer and new crop varieties spawned a period of increased productivity unparalleled in agricultural history. This century also saw the introduction of new chemical tools to assist farmers in controlling a myriad of pests (insects, weeds, and fungi) which continued to hamper food and fiber production efforts. Prior to the introduction of these new tools, various types of chemical control agents had been used for many years in the production of some fruits and vegetables.The new, highly effective, synthetic organic chemicals (pesticides) introduced a whole new level of performance and found ready acceptance in nearly all crop production systems. These production practice changes have allowed US farmers to provide the cheapest, most abundant, and highest quality food supply of any nation in the world.

The practical utility of pesticides stemmed from the selective chemical toxicity that existed between the crop and the pest controlled. Since pesticides had the potential to be toxic to other organisms, rules governing their use were quickly introduced. Ultimately the Federal Insecticide, Fungicide, and Rodentacide Act (FIFRA) and the Federal Food, Drug, and Cosmetic Act (FFDCA) were enacted into law to regulate this growing agrochemical industry and to monitor the testing required to register a new pesticide. The need for these regulations was based on the awareness that some toxicologically significant residues and metabolites remained on or in the harvested crops that were to be used for food or feed. FIFRA dictated that safe tolerance levels [amount of residue in parts per million (ppm) in/on farm commodities as they leave the farm gate] would be established for these residues, thereby ensuring public safety. FFDCA, among other things, assured the safety of processed foods by establishing safe tolerance limits for pesticide residues in processed foods. The rules and interpretation of the rules were not always consistent between these two government offices.

Pesticide registration and use in the USA are regulated by the EPA OPPTS. The regulations are found in the Food and Drug Administration (FDA) Code of Federal Regulations Title (CFR) 40 Parts 152 through 189(1). These guidelines have been revised and updated as new advances in toxicology increased our understanding of the toxic risk pesticides posed. The development of highly selective and extremely potent pesticides has encouraged tremendous strides in the capability of analytical chemistry methods associated with detecting residues in farm commodities. These parallel advances in toxicology and analytical chemistry have strengthened the assurance that pesticides can be used safely and efficiently in our farm production programs. The most recent revisions of the testing guidelines occurred in August 1996 when OPPTS published a unified, consolidated, and correlated new 'how-to' guideline entitled 'Residue Chemistry Test Guidelines'. The intent of the new guideline was to harmonize testing procedures for residue chemistry, which includes generating and analyzing field residue samples. The analytical results indicate the amount of pesticide residue remaining in samples at harvest or after processing and are used in setting pesticide tolerances in food and feed and in evaluating dietary exposure potential. The second recent change was the passage of the FQPA in 1996. The FQPA brought tolerance setting in farm commodities and processed foods under the same tolerance setting guidelines. The FQPA dictated the use of a science-based tolerance setting process for the entire food production system. This was the most significant aspect of this regulation as it pertains to field residue trials. Finally, FQPA dictated that tolerances and overall guidelines be periodically evaluated for relevance as the industry and tools change. Another significant change in recent years is the advent of the Internet. Current regulatory information can readily be accessed from many sources even prior to formal publication. A few of the most useful sites relative to planning and conducting field residue studies are listed below:

United States Department of Agriculture (USDA)/National Agricultural Statistical Service (NASS) crop production and usage estimates.

NASS home page: usda.gov/nass/

EPA OPPTS crop matrix menu: epa.gov/oppbead1/matrices/ matrixmenu.htm

National Center for Food and Agricultural Policy: ncfap.org/ default.htm

EPA Registration Eligibility Decisions (REDs) and Interim Reregistration Eligibility Decisions (IREDs) epa.gov/pesticides/reregistration/ status.htm

EPA OPPTS REDs: epa.gov/oppsrrd1/op/

EPA Food and Feed Crop Dictionary: epa.gov/opphed01/foodfeed/-old/lookatX.htm

Additionally, commodity groups, CropLife America [(CLA), formerly American Crop Protection Association (ACPA)], the Chemical Manufacturers Association (CMA), and the USDA are excellent sources of information relative to current regulatory activities which will impact both production agriculture and the setting of tolerances to ensure food safety. The purpose of this article is to summarize the key impacts of the 1996 OPPTS 860 Residue Chemistry Test Guideline series as they impact research associated with field production of RAC samples to be used in establishing safe tolerance limits for pesticides used in commercial agricultural production.

2 Description of the different types of field crop residue studies

Residues of pesticides may be found in many places following the application(s) of a pesticide to a crop. Pesticide residues are commonly found on the surface or inside the tissue of treated crops. Residues may be found in the soil in which the crop was grown. The soil residual materials may arise via either direct application to the soil or from left over plant litter (straw, culls, etc.) which was incorporated into the soil in preparation for the new crop. Residue may be found in following or rotational crops when significant residue remained or accumulated in the soil associated with the treated crop. Residues may also appear in the atmosphere if the product is highly volatile or carried over as spray drift deposits. Finally, residues may appear in run-off water following heavy rain or irrigation or in groundwater if the product and/or its degradation products are highly water-soluble. EPA has established specific testing procedures to address the concentration of the ai (parent molecule), metabolic products, and chemical degradation products in the various environmental compartments following the use of a pesticide in the production of a crop. This article will only deal with the residues that are found on or in the plant tissue that will be used for food or feed.

All RACs produced by each crop must be analyzed when establishing a crop tolerance. Specific RAC samples for residue testing have been identified for each crop. The primary commodities include all of the plant parts that may be consumed by people or fed to animals. For example, RAC samples may come from fruits, vegetables, grain, forage, hay, straw, stover, roots, tubers, stollons, bulbs, nut meats, berries, spears, leaves, leaf sprouts, and flower heads. However, the exact samples to be considered in a residue study can be influenced by the label use pattern associated with a specific pesticide and crop. If a pesticide is only applied late in the season, RAC samples that develop prior to the application of the pesticide may not require a tolerance be established. Some crop RACs are commonly converted to processed commodities prior to being eaten (e.g., raisins, grain starch, flour, etc.). Some processing procedures yield by-products that are fed to animals (e.g., raisin waste, wet apple pomace, cotton gin by-products, almond hulls, potato waste, etc.). Residue tolerances, therefore, must be established for each RAC and, where applicable, each processed commodity and/or associated processed by-product.

2.1 EPA guidelines and requirements

The guidelines for field residue trials currently in effect are included in the 'Residue Chemistry Test Guidelines'. The guidelines consist of 17 chapters or sections each dedicated to specific aspects of the residue chemistry activities associated with obtaining pesticide residue data. For convenience throughout the remainder of this article, these guidelines will be referred to as the 860.Series or as the section number in the series. The actual titles for each of the sections in the 860.Series testing guidelines are as follows:

OPPTS 860.1000 Background

OPPTS 860.1100 Chemical Identity

OPPTS 860.1200 Directions for Use

OPPTS 860.1300 Nature of Residue - Plants, Livestock

OPPTS 860.1340 Residue Analytical Method

OPPTS 860.1360 Multiresidue Method

OPPTS 860.1380 Storage Stability Data

OPPTS 860.1400 Water, Fish, Irrigated Crops

OPPTS 860.1460 Food Handling

OPPTS 860.1480 Meat/Milk/Poultry/Eggs

OPPTS 860.1500 Crop Field Trials

OPPTS 860.1520 Processed Food/Feed

OPPTS 860.1550 Proposed Tolerances

OPPTS 860.1560 Reasonable Grounds in Support of the Petition

OPPTS 860.1650 Submittal of Analytical Reference Standards

OPPTS 860.1850 Confined Accumulation in Rotational Crops

OPPTS 860.1900 Field Accumulation in Rotational Crops.

There are important instructions in each section in the series relative to specific types of tests. However, four sections of the series provide particularly significant instructions relative to field crop residue trials and a short summary of their content is listed below.

2.1.1 OPPTS 860.1000 Background

This section outlines the general intent of the Residue Chemistry Guideline Series and serves as the basic starting point for each of the other sections in the series. In this section the following can be found:

1. purpose and scope of data requirements;

2. regulatory authority upon which the guideline is established;

3. instructions for minor change in use pattern;

4. definition of and instructions for food use/nonfood use determinations;

5. instructions relative to tobacco use tolerances;

6. considerations for aquatic uses;

7. special considerations and data requirements for temporary tolerances;

8. instruction for presentation of residue data;

9. guidance on submittal of raw data, and references.

Table 1 of this guideline defines the RACs and processed commodities associated with each crop. There is an extensive footnote section to Table 1 that provides considerable additional detail about the crop matrices defined in the table. Table 1 also indicates the percentage of an animal's diet that a particular RAC or processed commodity must contain if an animal feeding study should be required. The instructions in this section of the guideline should be reviewed early in the planning phase of any crop field residue study.

2.1.2 OPPTS 860.1500 Crop Field Trials

This section outlines the considerations and priorities that were used by the EPA to establish field test guidelines. This section identifies important factors to be addressed in the design, conduct, and reporting of field residue trials. Table 1 indicates the minimum number of trials to conduct and samples to collect in a crop field residue study. The definition and use of crop groups to reduce the field testing cost are outlined in Tables 2-4. At the end of this section is a map that divides the USA into 13 testing or crop production regions, each region representing a fairly uniform farm production environment. This map has been extended into Canada [HED SOP 98.2 Supplementary Guidance on Use of OPPTS Residue Chemistry Test Guideline 860.1500 (residue zone maps - Canadian extension) 4/8/98] and efforts are under way to extend the map into Mexico. The EPA cropping regions in which to locate field residue trials in a study are listed in Table 5. Other important items discussed in OPPTS 860.1500 include:

1. the location of the individual trials within EPA cropping regions;

2. the range of application rates and sample timings that must be included in the study;

3. how special local needs may be met;

4. the amount of crop or crop fraction that must be collected to be a representative sample.

Trial number and location and definition of specific crop fractions to be sampled had been a significant reason for study rejection prior to 1996. This particular guideline has helped resolve these issues in studies conducted since that time.

2.1.3 OPPTS 860.1520 Processed Food/Feed

Pesticide residues may be found on the surface of the plant material, or they may be selectively absorbed/translocated inside the tissue. Processing studies are required to determine whether residues degrade or concentrate during typical food processing activities. If residues concentrate during the processing procedures, then a tolerance will be needed for residues in that processing commodity. If residues degrade or do not concentrate, the tolerance for the RAC will be assigned to the food and feed derived from the RAC. Several important instructions relative to the conduct of a processing study as well as preparing and presenting the data from the study are found in this guideline. Additionally, this section provides instructions on how to apply the data to a proposed tolerance when residues are found to concentrate in the processed fractions. Careful attention to the details in this guideline is necessary if a successful processing study is to be conducted.

2.1.4 OPPTS 860.1900 field accumulation in rotational crops

If the confined rotational crop study indicates a potential for residues to persist in the soil and are detected in crops grown as a rotational crop following a treated crop, then a field accumulation study must be conducted. This study is often referred to as a field crop rotation study. The field crop rotation study will provide the data necessary to establish rotational intervals that will limit or prevent residue accumulation in rotational crops.


Excerpted from Handbook of Residue Analytical Methods for Agrochemicals, 2 Volume Set Copyright © 2003 by John Wiley & Sons Ltd.. Excerpted by permission.
All rights reserved. No part of this excerpt may be reproduced or reprinted without permission in writing from the publisher.
Excerpts are provided by Dial-A-Book Inc. solely for the personal use of visitors to this web site.

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