Handbook of Residue Analytical Methods for Agrochemicals VOLUME 1 and VOLUME 2 doc

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Handbook of Residue Analytical Methods for Agrochemicals VOLUME and VOLUME Editor-in-Chief Dr Philip W Lee DuPont Crop Protection USA Copyright C 2003 John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex PO19 8SQ, England Telephone (+44) 1243 779777 Email (for orders and customer service enquiries): cs-books@wiley.co.uk Visit our Home Page on www.wileyeurope.com or www.wiley.com All Rights Reserved No part of this publication may be reproduced, stored in a retrieval system or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning or otherwise, except under the terms of the Copyright, Designs and Patents Act 1988 or under the terms of a licence issued by the Copyright Licensing Agency Ltd, 90 Tottenham Court Road, London W1T 4LP, UK, without the permission in writing of the Publisher Requests to the Publisher should be addressed to the Permissions Department, John Wiley & Sons Ltd, The Atrium, Southern Gate, Chichester, West Sussex PO19 8SQ, England, or emailed to permreq@wiley.co.uk, or faxed to (+44) 1243 770620 This publication is designed to provide accurate and authoritative information in regard to the subject matter covered It is sold on the understanding that the Publisher is not engaged in rendering professional services If professional advice or other expert assistance is required, the services of a competent professional should be sought Other Wiley Editorial Offices John Wiley & Sons Inc., 111 River Street, Hoboken, NJ 07030, USA Jossey-Bass, 989 Market Street, San Francisco, CA 94103-1741, USA Wiley-VCH Verlag GmbH, Boschstr 12, D-69469 Weinheim, Germany John Wiley & Sons Australia Ltd, 33 Park Road, Milton, Queensland 4064, Australia John Wiley & Sons (Asia) Pte Ltd, Clementi Loop #02-01, Jin Xing Distripark, Singapore 129809 John Wiley & Sons Canada Ltd, 22 Worcester Road, Etobicoke, Ontario, Canada M9W 1L1 Wiley also publishes its books in a variety of electronic formats Some content that appears in print may not be available in electronic books Where articles in the Handbook of Residue Analytical Methods for Agrochemicals have been written by government employees in the United States of America, please contact the publisher for information on the copyright status of such works, if required Works written by US government employees and classified as US Government Works are in the public domain in the United States of America Preface The agrochemical industry is, globally, one of the most heavily regulated industries today Extensive product chemistry, environmental fate, residue chemistry, ecotoxicology, and mammalian toxicology data are required to support the registration and reregistration of all crop protection products This information is used not only to conduct human dietary and worker exposure risk assessments but also to determine the potential impact of the agrochemicals and their degradation products/metabolites on the environment and sensitive ecosystems The quality of the residue data, including the reliability and sensitivities of the analytical methods and the validity of the collected biological/environmental samples, is critical to the acceptability and validity of the risk characterization/assessment Differences in testing guidelines between the various regulatory authorities and the lack of standardization in test method specifications further complicate the interpretation and broad application of the exposure data Significant progress has been achieved in residue analytical technology in the past 50 years Today’s residue analytical methodology detects multiple analytes routinely at the nanogram per kilogram (ppt) level in a wide variety of sample matrices with a high level of selectively and accuracy The role of the residue analytical chemist is no longer limited to the development and validation of analytical methods but also includes design and conduct of complex field crop residue and environmental monitoring studies This is a real challenge, especially when studies are conducted under the strict Good Laboratory Practices guidelines Recognizing the diverse and rapid growth of residue chemistry as an important scientific discipline, Dr Terry Roberts, Founding Editor of the Handbook of the Residue Analytical Methods of Agrochemicals, organized this publication effort in 1999 The editorial team includes Dr Hiro Aizawa (Hiro Research Consultancy), Dr Al Barefoot (DuPont Crop Protection) and Dr John Murphy (Bayer CropScience) The scope/objective of this handbook is to present to the reader a comprehensive overview of current global regulatory requirements and the application of various analytical technologies (chromatographic and non-chromatographic) to residue analysis Best practices to conduct various crop residue and field monitoring studies and detailed method procedures for the determination of major classes of agrochemicals, as well as individual compounds, are key components of this handbook This handbook consists of two volumes and approximately 80 individual chapters The editorial team acknowledges the high quality of the contributions from the regulatory, academic, and industrial researchers around the world It is their commitment in time and effort that make this a successful publication project Each chapter was reviewed by at least one editor and often by other technical experts The editorial team acknowledges the generous advice and reviews provided by our colleagues from DuPont Crop Protection (Dr Wynn John, Dr Chuck Powley) and Bayer CorpScience (Dr Lou Russo), the US EPA (Dr Alex Krynitsky) and the USDA ARS (Dr David Smith) We would also appreciate comments, feedback and upgrades from the readers, so that correction and improvement can be made for later editions or printings xlii Preface The editorial team is also grateful for the valuable support from the Publisher (John Wiley & Sons Ltd.), in particular Ms Lynette James, and from the Project Manager (Gray Publishing), in particular Ms Lesley Gray, for their efficient coordination during the planning, review and production phase of this publication effort Finally, this handbook is dedicated to all past and present residue analytical chemists It is their vision and creativity that continues to push back the frontier of residue analytical technology Philip W Lee Newark, Delaware December, 2002 Editorial Board Editor-in-Chief Dr Philip W Lee DuPont Crop Protection Stine-Haskell Research Center Newark Delaware USA Associate Editors Professor Hiroyasu Aizawa Hiro Research Consultancy Inc.(HRCI) Tokyo Japan Dr Aldos C Barefoot DuPont Crop Protection Stine-Haskell Research Center Newark Delaware USA Founding Editor Dr Terry Roberts Anglesey North Wales UK Dr John J Murphy Dietary Exposure Bayer CropScience Stilwell Kansas USA List of contributors Lutz Alder Federal Institute for Health Protection of Consumers and Veterinary Medicine (BgVV), Berlin, Germany Todd A Anderson Texas Tech University, Lubbock, TX, USA Reiner Bacher PTRL Europe GmbH, Ulm, Germany Johannes Corley Rutgers, The State University of New Jersey, North Brunswick, NJ, USA Kay K Curry Technology Sciences Group Inc., Washington, DC, USA William J Englar Englar Food Laboratories, Inc., Moses Lake, WA, USA Michael R Barrett United States Environmental Protection Agency, Washington, DC, USA Cheryl M Englar-Coulter Englar Food Laboratories, Inc., Moses Lake, WA, USA Elizabeth Behl United States Environmental Protection Agency, Washington, DC, USA Neal Ewing CA, USA Kimberly S Billesbach Bayer CropScience, Stilwell, KS, USA John Fuhrman James F Brady Syngenta Crop Protection, Inc., Greensboro, NC, USA David J Brookman Technology Sciences Group Inc., Washington, DC, USA Thomas J Burnett Eli Lilly and Company, Greenfield, IN, USA Maria Elena Y Cabusas DuPont Crop Protection, Newark, DE, USA Leslie S Carver Waterborne Environmental, Inc., Leesburg, VA, USA Andrey Chen FMC, Princeton, NJ, USA Joseph R Chepega Waterborne Environmental, Inc., Leesburg, VA, USA Mihai Cicotti Switzerland Battelle Memorial Institute, Geneva, National Food Laboratory, Inc., Dublin, Monsanto, St Louis, MO, USA Richard J Fussell Central Science Laboratory, York, UK Willa Garner GARNDAL Associates, Inc., Mount Airy, MD, USA Shirley J Gee USA University of California, Davis, CA, Thomas J Gould Bayer CropScience, Stilwell, KS, USA Timothy J Grace USA Bayer CropScience, Stilwell, KS, Charles A Green Valent USA Corporation, Dublin, CA, USA Amy Hackett Monsanto, St Louis, MO, USA Bruce D Hammock CA, USA University of California, Davis, Thomas J Class PTRL Europe GmbH, Ulm, Germany Ralf Hă nel Federal Biological Research Centre for a Agriculture and Forestry (BBA), Braunschweig, Germany George P Cobb USA Vincent Hebert WA, USA Texas Tech University, Lubbock, TX, Washington State University, Richland, xliv List of contributors Andrew J Hewitt Stewart Agricultural Research Services, Macon, MO, USA James S LeNoir DuPont Crop Protection, Newark, DE, USA Richard Honeycutt H.E.R.A.C., Inc., Greensboro, NC, USA Yi Lin USA Mitsumasa Ikeda Kumiai Chemical Industry Co., Ltd, Shizuoka, Japan Cynthia Lipton Yuji Ikemoto Nihon Nohyaku Co Ltd, Osaka, Japan Syngenta Crop Protection, Inc., Greensboro, NC, Byotix, Inc., Richmond, CA, USA Joseph H Massey Mississippi State University, Starkville, MS, USA Fujio Ishijima Hokko Chemical Industry Co Ltd, Kanagawa, Japan Greg C Mattern USA Scott H Jackson BASF Corporation, Research Triangle Park, NC, USA Joseph P McClory DE, USA Kathryn M Jernberg DuPont Crop Protection, Newark, DE, USA Carolyn Mentzer MD, USA William W John DuPont Crop Protection, Stine Haskell Research Center, Newark, DE, USA D Larry Merricks MD, USA Setsuko Katsurada Sankyo Co Ltd, Shiga, Japan Sean M Moore Guenther Kempe Landesuntersuchungsanstalt, Chemnitz, Germany Kouji Nakamura Saitama Prefecture Agriculture and Forestry Research Center, Kuki, Japan Douglas E Kiehl Eli Lilly and Company, Greenfield, IN, USA Kazuo Ogura Agricultural Chemicals Inspection Station, Tokyo, Japan Philip James Kijak US Food and Drug Administration, Laurel, MD, USA Jeff Old Alexander J Krynitsky US Environmental Protection Agency, EPA Environmental Science Center, Fort Meade, MD, USA Chung K Lam Bayer CropScience, Stilwell, KS, USA DuPont Crop Protection, Newark, Agrisearch Incorporated, Thurmont, Agrisearch Incorporated, Frederick, Bayer CropScience, Stilwell, KS, USA Inveresk Research, Tranent, UK Takeo Otsuka Hiroko Kobayashi Research Institute of Japan Plant Protection Association, Ibaraki, Japan Bayer CropScience, Stilwell, KS, Sankyo Co Ltd, Shiga, Japan John C Peterson Englar Food Laboratories, Inc., Moses Lake, WA, USA Beth M Polakoff USA Exponent, Inc., Washington, DC, Charles R Powley DuPont Crop Protection, Newark, DE, USA Steven J Lehotay USDA Agricultural Research Service, Eastern Regional Research Center, Wyndmoor, PA, USA Robin S Readnour IN, USA William M Leimkuehler Bayer CropScience, Stilwell, KS, USA Valerie B Reeves US Food and Drug Administration, Rockville, MD, USA Eli Lilly and Company, Greenfield, List of contributors xlv Stewart L Reynolds Central Science Laboratory, York, UK Guy R Stehly USGS, Biological Resources Division, La Crosse, WI, USA Neil J Robinson Syngenta, Bracknell, UK Shigeji Sugimoto Janine E Rose Manabu Toujigamori PTRL West, Inc., Hercules, CA, USA Nippon Soda Co Ltd, Tokyo, Japan Sankyo Co Ltd, Shiga, Japan Louis Russo USA Bayer CropScience, Kansas City, MO, Yasuhiro Tsujino Mariko Sabi Sankyo Co Ltd, Shiga, Japan Michael P Turberg Eli Lilly and Company, Greenfield, IN, USA Shingo Sadakane Sankyo Co Ltd, Shiga, Japan Manasi Saha BASF Corporation, Research Triangle Park, NC, USA Takashi Saito Sankyo Co Ltd, Shiga, Japan Yoshihiro Saito Shizuoka, Japan Kumiai Chemical Industry Co., Ltd, Thomas Schreier Valent USA Corporation, Dublin, CA, USA James N Seiber Western Regional Research Center, USDA Agricultural Research Service, Albany, CA, USA Robert J Seymour Bayer CropScience, Research Triangle Park, NC, USA Guomin Shan Dow AgroSciences LLC, Indianapolis, IN, USA Weilin L Shelver US Department of Agriculture, Agricultural Research Service, Fargo, ND, USA Johannes Siebers Federal Biological Research Centre for Agriculture and Forestry (BBA), Braunschweig, Germany David J Smith US Department of Agriculture, Agricultural Research Service, Fargo, ND, USA Craig A Smitley NC, USA Takashi Ueda Sankyo Co Ltd, Shiga, Japan Sankyo Co Ltd, Shiga, Japan Masako Ueji National Institute for Agro-Environmental Sciences, Tsukuba, Japan Noriharu Umetsu Otsuka Chemical Co Ltd, Naruto, Japan David L Valcore USA Dow AgroSciences, Indianapolis, IN, Chantel Van Bellinghan Monsanto, Brussels, Belgium Michael F Wilson Central Science Laboratory, York, UK James E Woodrow University of Nevada, Reno, NV, USA Akira Yagi Kumiai Chemical Industry Co., Ltd, Shizuoka, Japan Katsura Yagi Otsuka Chemical Co Ltd, Naruto, Japan Hisayoshi Yamagishi Research Institute of Japan Plant Protection Association, Ibaraki, Japan Hiroki Yamamoto Japan Shimane University, Matsue, Robert A Yokley Syngenta Crop Protection, Inc., Greensboro, NC, USA Scynexis, Research Triangle Park, Lisa D Spurlock-Brouwer Eli Lilly and Company, Greenfield, IN, USA Sabrina X Zhao Pfizer Inc., Groton, CT, USA Eberhard Zietz Institut Fresenius, Taunusstein, Germany Contents of Volume 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 xli xliii 1 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 Hă nel a 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 13 13 14 14 14 15 18 18 20 20 21 23 23 27 31 32 33 34 35 36 36 vi Contents of Volume 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 t99 sLLMV method Confirmation Representative data Conclusions Acknowledgements References 38 38 40 41 41 41 46 47 47 48 49 49 50 50 51 51 52 53 54 54 55 55 57 58 58 59 59 61 63 63 66 67 67 68 70 71 72 73 74 74 83 Index Terms stability airborne pesticides monitoring samples foodstuffs freezer storage groundwater parameters NADA methods spray drift study tracers storage test substance triazine samples stable isotopes stagnant water Standard Operating Procedures (SOPs) airborne pesticides monitoring animal drug residue methods animal health drugs calibration electronic record keeping field trials large-scale market basket surveys processing standard treatments, spray drift studies standardization CEN method validation Nordic country validation UK validation standards airborne pesticides monitoring American Society of Agricultural Engineers (ASAE) Standard S561 internal NADA method criteria starch, carfentrazone-ethyl starlings Diazinon 50W wildlife exposure case study Fortress-5G wildlife exposure case study statistical analyses, field soil dissipation studies STC see safe tissue concentrations Stehly, Guy R steroids stone fruit, pyriproxyfen storage animal health drugs antibodies electronic record keeping field soil dissipation study samples field trial samples field trials requirements foodstuffs Fortress-5G wildlife exposure case study samples Links 930 303 879 804 82 984 870 156 428 832 800 931 85 262 1042 1028 152 240 220 985 806 904 161 162 90 1042 162 1045 163 224 227 951 1048 175 952 110 119 115 930 977 833 83 475 950 953 880 248 285 1340 279 645 1063 867 154 189 302 953 1065 870 159 193 161 This page has been reformatted by Knovel to provide easier navigation 162 1055 199 1079 209 84 Index Terms storage (cont.) groundwater samples impact assessments Japanese crop residue studies large-scale market basket surveys NADA methods processing stability test substances, worker exposure and re-entry studies triazine samples UK single-laboratory validation wildlife exposure assessment samples worker exposure and re-entry study samples stover carfentrazone-ethyl sulfentrazone straw cereal, famoxadone rice benfuracarb bispyribac-sodium carfentrazone-ethyl mepronil prohexadione-calcium pyriminobac-methyl sulfentrazone wheat carfentrazone-ethyl flucarbazone-sodium strawberries acetamiprid azoxystrobin hexythiazox imibenconazole mepanipyrim milbemectin prohexadione-calcium pyrimidifen terbacil streptomycin string beans, mepronil strings, spray drift study samplers strobilurins study designs environmental fate studies in rice paddy fields field soil dissipation studies spray drift studies wildlife exposure assessments worker exposure and re-entry studies see also experimental designs Links 808 618 46 240 82 225 870 998 428 118 945 998 879 904 1007 1015 1023 475 564 1177 1263 469 475 1228 532 551 564 475 489 1242 1167 1316 1215 1221 1331 532 1336 578 690 1228 981 1167 703 894 853 975 939 991 This page has been reformatted by Knovel to provide easier navigation 85 Index Terms Study Directors animal health drugs electronic record keeping field trials large-scale market basket surveys processing wildlife exposure assessments study documentation see documentation study objectives environmental fate studies in rice paddy fields spray drift studies wildlife exposure assessments study plans see planning study protocols see protocols study reports see communication; reports study sites see sites styrene-divinylbenzene sub-soil markers subcritical fluid extraction submissions subplots, field soil dissipation studies subsampling suction lysimeters sudachi, mepanipyrim sugar processing sulfentrazone sugar beet alanycarb azoxystrobin benfuracarb hymexazol mepronil sugar cane flumioxazin isoxathion sulfentrazone terbacil Sugimoto, Shigeji suitability see system suitability sulfachloropyridazine sulfadimethoxine analysis immunoaffinity chromatography immunoassay ultrafiltration sulfadimidine Links 260 1031 173 235 224 940 192 194 226 229 894 975 940 826 857 434 606 854 163 812 1221 1066 218 564 1250 1167 1263 1211 1228 502 1327 564 578 38 316 316 708 704 310 704 This page has been reformatted by Knovel to provide easier navigation 203 86 Index Terms sulfamethazine analysis animal health drugs immunoaffinity chromatography tolerances sulfanilamides sulfates sulfathiazole sulfentrazone sulfentrazone-3-carboxylic acid (SCA) sulfometuron methyl sulfonamides animal health drugs flucarbazone-sodium metabolite immunoaffinity chromatography immunoassay sulfonic acid sulfonylureas analytical methodology class characteristics crops, food and feed HPLC/MS immunoassay LC/MS/MS analysis soil water sulfosulfuron summer oranges, milbemectin summer squash, pyriproxyfen sunflowers benfuracarb sulfentrazone supercritical fluid extraction (SFE) animal health drugs foodstuffs immunoassay pesticides soil extraction triazine compounds supersonic molecular beam mass spectrometry (SMBMS) supplemental files supplemental irrigation supply wells surface plasmon resonance (SPR) surface soil preparation samplers Links 316 259 708 690 57 286 316 564 565 403 257 490 708 700 490 400 402 400 405 780 722 401 407 408 404 1331 1340 264 704 259 704 708 404 259 290 704 402 409 1263 564 287 306 696 758 875 428 763 1069 848 799 670 861 966 729 704 432 435 803 967 This page has been reformatted by Knovel to provide easier navigation 442 87 Index Terms surface water EU enforcement method validation field trials impact assessments isoxaflutole matrix effects residue limit EU legislation surveys suspended solids SW see water solubility sweet corn benfuracarb carfentrazone-ethyl tebuconazole system life cycle system qualification system suitability T T1/2, versus DT50 t99sLLMV method tall crops, field trials tandem mass spectrometry (MS/MS) calibration curves field soil dissipation study samples foodstuffs oxime carbamates pesticides residues in water sulfonylurea herbicides tepraloxydim triazine compounds water samples TaqMan target crops target spray volume target tissues TC TCDD see 2,3,7,8-tetrachlorodibenzo-p-dioxin TDR see time domain reflectometry tea acetamiprid alanycarb buprofezin crop grouping fenpyroximate hexythiazox isoxathion pyrimidifen tebuconazole tebufenozide Links 29 151 610 509 832 18 231 903 1263 475 1233 1056 1038 82 883 70 144 833 878 736 1146 762 831 401 878 440 829 666 846 862 691 275 1242 1250 1270 172 1308 1316 1327 1336 1100 766 613 615 620 1062 73 74 741 1148 742 402 409 441 834 445 110 112 173 1118 1120 This page has been reformatted by Knovel to provide easier navigation 1124 1233 88 Index Terms Technical Committee (TC) Tedlar bags Teflon strands temperature, recoveries from water template DNA tepraloxydim terbacil terbutaline terbuthylazine terbutryn terbutryne test plots see plots test sites see sites test substances animal health drugs characterization dislodgeable foliar residue studies fate studies in rice paddy fields field soil dissipation study applications field trials formulations receipt and storage tracking wildlife exposure assessments test systems dislodgeable foliar residue studies wildlife exposure assessments testing strategy, field trials 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) tetrachloroterephthalate tetraconazole, multi-residue methods tetracyclines chromatography immunoassay oxytetracycline 3,7,9,13-tetramethyl-5,11-dioxa-2,8,14-trithia-4,7,9,12tetraazapentadeca-3,12-diene-6,10-dione see thiodicarb thenylchlor thermal cycling thermospray (TSP) thiabendazoles immunoassay multi-residue methods thiacloprid crop samples soil samples water samples Links 275 911 914 824 659 878 578 688 413 413 745 265 153 963 895 861 145 184 997 1051 941 110 912 112 921 689 434 153 179 962 942 140 620 1101 635 637 1118 1120 312 690 273 705 310 690 707 1121 203 1125 1124 585 661 829 695 1101 1128 1138 1141 This page has been reformatted by Knovel to provide easier navigation 89 Index Terms thiamethoxam crop samples LC/MS methods soil samples water samples thiamphenicol thiazoles thiazolidinone acaricides thienylchlor thifensulfuron-methyl thifluzamide thiodicarb food/tissue samples HPLC/MS methods soil samples water samples thiofanox food/tissue samples HPLC/MS methods soil samples water samples thiuram disulfide throughput, analytical method development thyroglobulin time domain reflectometry (TDR) time issues analytical method development field soil dissipation study applications sample preparation see also sampling time-averaged sampling time-of-flight mass spectrometry (TOFMS) Timme-Frehse-Laska equation Tinopal CBS-X tissue animal health drugs azoxystrobin carfentrazone-ethyl EU data generation method validation EU enforcement method validation fenoxycarb immunoassay oxime carbamates triazine herbicides wildlife exposure assessments tissues, analytical method development tobacco alanycarb benfuracarb cyfluthrin Links 1128 766 1138 1141 315 1101 1316 345 401 733 1153 776 1158 1151 1153 1144 1158 1151 114 54 639 886 1121 1124 403 404 777 1144 1159 1159 54 849 837 910 736 882 977 250 1167 475 34 31 1294 691 1153 435 939 53 741 763 693 1250 1263 1282 This page has been reformatted by Knovel to provide easier navigation 745 90 Index Terms tobacco (cont.) flumetralin hymexazol sulfentrazone TOFMS see time-of-flight mass spectrometry tolerances crop grouping foodstuffs guidelines immunoassay NADA method analyte selection neonicotinoids rotational crops validation see also maximum residue limits tomatoes acetamiprid azoxystrobin benfuracarb buprofezin cyfluthrin famoxadone flutolanil imibenconazole mepanipyrim oxamyl processing pyriproxyfen tebuconazole topography total toxic residue (TTR) total vegetation control (TVC), carfentrazone-ethyl toxic transformation products ‘trace enrichment’ tracers haptens spray drift studies trade associations training, personnel tralkoxydim trans-dermal ruminal cannulation transects transfer coefficient data translation of documents transportation field trials Fortress-5G wildlife exposure case study samples groundwater samples impact assessments Japanese crop residue studies Links 498 1211 564 141 300 136 681 80 1129 140 762 1242 1167 1263 1270 1282 1177 1198 1215 1221 964 217 1340 1233 859 162 475 940 825 636 976 220 179 766 270 943 960 206 152 953 808 618 46 137 688 966 968 972 207 210 239 941 1048 160 187 190 203 209 984 This page has been reformatted by Knovel to provide easier navigation 212 91 Index Terms transportation (cont.) large-scale market basket surveys processing rice paddy field fate samples wildlife exposure assessment samples worker exposure and re-entry study samples trapping efficiency trapping grids travel fortification samples treated plots tree nuts, fenoxycarb triadimefon triadimenol trials see field trials triapenthenol triasulfuron triazbutil triazine herbicides air biological fluids crops, food, feed and animal tissues future of analysis HPLC/MS immunoassay instrumentation overview physical data soil analytical methodology structures water analytical methodology see also individual compounds triazole fungicides imibenconazole tebuconazole triazoxide tribenuron-methyl acid-sensitivity electrophoresis LC/MS/MS analysis structure 1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane see DDT 2,4,6-trichlorophenyl 4-aminophenyl ether (CNP-NH2) plant analysis soil analysis water analysis trietazine triflumizole α,α,α,-trifluoro-3'-isopropoxy-o-toluanilide see flutolanil 2-(trifluoromethyl)benzanilide moiety Links 240 225 902 945 1014 916 943 1015 854 1294 1101 1101 1101 404 1101 412 438 437 435 443 780 636 439 412 412 429 413 416 1215 1233 1101 1015 1023 1119 1119 1120 1120 1124 1124 1118 724 1120 1120 1124 1124 695 413 1121 1126 405 745 403 401 408 455 461 462 413 1101 456 458 1118 1121 1199 This page has been reformatted by Knovel to provide easier navigation 1126 92 Index Terms trifluralin dinitroaniline characteristics plant material analytical methodology soil analytical methodology soil metabolites structure trifluroacetylation triflusulfuron methyl trimethoprim trinexapac-ethyl trip blanks trip spikes triticonazole trueness, method validation TSP see thermospray TTR see total toxic residue tulobuterol Turberg, Michael P turbutryn see terbutryn turf grass, alanycarb TVC see total vegetation control two dimensional GC (GC x GC) two-step approach, limit of detection U Ueji, Masako UK see United Kingdom ultrafiltration ultrasonication see also sonication ultraviolet (UV) detectors under-application uniconazole United Kingdom (UK), single-laboratory validation United States agencies/organizations animal drug residue methods for Food and Drug Administration field trials United States Department of Agriculture (USDA) animal health drugs field trials foodstuffs GM crops Grain Inspection Protection Service (GIPSA) large-scale market basket surveys PPQ forms United States Geological Survey (USGS) units of weight unsaturated zone sampling Unshu oranges, mepanipyrim Links 389 391 395 397 390 461 403 690 590 810 930 1101 21 392 393 394 404 405 406 1118 113 1120 1124 738 67 70 73 389 451 310 431 436 689 248 1250 828 155 1101 115 829 156 1120 1124 200 201 615 619 76 135 248 136 300 653 630 234 209 613 812 1221 This page has been reformatted by Knovel to provide easier navigation 209 93 Index Terms Links upland use pattern uracil herbicides, terbacil urea metabolites, imidacloprid urine triazine analysis wildlife exposure assessments 848 578 1320 worker exposure and re-entry studies US see United States USA see United States USDA see United States Department of Agriculture use patterns field soil dissipation studies field trials test substances in rice paddy fields USEPA see Environmental Protection Agency User Acceptance Testing USGS see United States Geological Survey UV see ultraviolet V vaccines see animal health drugs vacuum manifolds Valcore, David L validation animal drug residue methods CEN methods data generation methods deviation from good analytical practice dislodgeable foliar residue studies analysis methods electronic record keeping enforcement analytical methods environmental fate studies in rice paddy fields EU member state methods evaluation of submitted methods extraction immunoassay impact assessments polymerase chain reaction tolerances Van Bellinghan, Chantel vapor density vapor pressure (VP) airborne pesticides characteristics design of field soil dissipation studies trapping efficiency of polymeric microporous adsorbents vapor sampling vapor/aerosol distribution variability fate studies in rice paddy fields field soil dissipation studies wildlife exposure assessments 1015 1020 845 144 895 177 437 939 1055 824 974 50 76 110 31 105 969 1032 25 904 94 21 758 646 608 664 762 344 917 909 844 917 909 923 896 852 945 88 1055 26 23 691 696 919 919 917 906 This page has been reformatted by Knovel to provide easier navigation 714 94 Index Terms vegetables crop grouping Directive 76/895/EEC fenoxycarb isoxathion see also individual types vegetation, bio-indicators vendor audits verification Nordic country validation performance vertical surface collectors veterinary drugs see animal health drugs vines vines (peanuts), flumioxazin violative residues virtual impactors volatile analytes volatilization agrochemicals from soil post-application volumetric water content volunteers, worker exposure and re-entry studies VP see vapor pressure W water alanycarb analytical method development anilide analytical methods azoxystrobin benfuracarb bispyribac-sodium buprofezin chloroacetanilide soil metabolites detection limits dinitroaniline analytical methodology diphenyl ether analysis environmental fate studies in rice paddy fields EU method validation EU residue limit legislation famoxadone fenoxycarb fenpyroximate field trials flucarbazone-sodium flumioxazin fluthiacet-methyl flutolanil historical perspective (pesticide analysis) HPLC/API-MS applications Links 171 17 1294 1327 982 1043 120 119 981 1250 502 258 914 58 843 924 884 998 1250 53 339 1167 1263 469 1270 349 833 398 461 892 29 18 1177 1294 1308 150 489 502 1191 1198 820 834 1044 121 130 300 916 1017 34 This page has been reformatted by Knovel to provide easier navigation 95 Index Terms water (cont.) HPLC/API-MS/MS applications imidacloprid isoxaflutole management practices matrix effects mepanipyrim neonicotinoids oxime carbamates preparation and instrumental analysis prodiamine pyraflufen-ethyl pyriproxyfen quality regulatory issues sample preparation subcritical sulfonylurea herbicides tebuconazole temperature effects on recoveries thenylchlor triazine analysis trinexapac-ethyl see also groundwater; surface water water balance, field soil dissipation studies water solubility (SW) water supply wells water-holding capacity (WHC) water-holding periods water-sensitive papers watermelons benfuracarb hymexazol imibenconazole mepanipyrim milbemectin watersheds weather conditions see meteorology; wind weathering, field fortifications weight units wells groundwater sampling volume calculation wet peel (potato), sulfentrazone WHC see water-holding capacity Links 834 1320 509 898 832 1221 1141 1151 818 526 540 1340 603 603 821 434 408 1233 824 585 416 590 884 843 799 886 893 980 1159 897 819 893 803 981 1263 1211 1215 1221 1331 615 1011 790 800 564 This page has been reformatted by Knovel to provide easier navigation 96 Index Terms wheat azoxystrobin carfentrazone-ethyl cyfluthrin flucarbazone-sodium isoxathion orbencarb prohexadione-calcium sulfentrazone whole-body analysis whole-body dosimetry field fortification preparation and storage field techniques simultaneous with biological monitoring wildlife exposure assessments best practices Diazinon 50W case study Fortress-5G case study study designs Wilson, M F wind airborne pesticides field soil dissipation studies field trials spray drift studies wind brakes, field trials wine famoxadone triazine analysis wipes background checks data field fortification simultaneous dosimetry-biological monitoring withdrawal period Wolt equation Woodrow, James E woody plants, alanycarb worker exposure data collection and field forms data issues dislodgeable foliar residue studies execution of field phase field methods observations of volunteers participants consent setting up field laboratories and equipment site selection storage and shipping of samples study designs and protocol preparation Links 1167 475 1282 489 1327 519 532 564 939 1007 1002 1018 936 948 952 939 727 925 862 144 977 144 151 978 173 981 1177 437 1005 1000 1024 1011 1019 251 883 908 1250 1022 1023 960 1000 989 1021 998 993 992 1023 991 This page has been reformatted by Knovel to provide easier navigation 192 983 97 Index Terms working range/linearity worksheets X XAD adsorbents Y Yamagishi, Hisayoshi Yamamoto, Hiroki Yokley, Robert A Youden test Z zearanol ‘zero tolerance’ zero-contamination sampling zero-day withdrawal zero-time concentrations Zietz, Eberhard zinc alkylenebis(dithiocarbamate) see zineb zineb Links 101 206 920 38 892 412 82 265 863 251 851 840 1089 866 867 1090 1091 This page has been reformatted by Knovel to provide easier navigation ... 12 13 12 14 12 14 12 14 12 15 12 15 12 16 12 16 12 16 12 17 12 17 12 17 12 17 12 18 12 19 12 19 12 19 12 19 12 20 12 21 12 21 122 2 12 22 12 22 12 23 12 23 12 23 12 24 12 24 12 25 12 25 12 25 12 26 12 26 12 26 12 27 12 27 xxxiii xxxiv... 12 28 12 28 12 28 12 29 12 29 12 30 12 30 12 30 12 30 12 31 12 31 12 31 123 2 12 32 12 32 12 33 12 33 12 34 12 34 12 35 12 35 12 35 12 35 12 36 12 36 12 36 12 37 12 38 12 38 12 39 12 40 12 41 124 2 12 42 12 43 12 43 12 43 12 43 12 44... 12 84 12 84 12 85 12 85 12 86 12 86 12 86 12 87 12 88 12 88 12 88 12 89 12 89 12 89 12 90 12 90 12 90 12 91 129 2 12 92 12 92 12 92 12 93 12 93 12 94 12 94 12 95 12 95 12 95 12 95 12 95 12 96 12 96 12 96 12 97 12 97 12 97 12 98 12 98

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  • 91942_toc.pdf

    • 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

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