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Residue Reviews / Ruckstands-Berichte: Residue of Pesticides and Other Foreign Chemicals in Foods and Feeds / Ruckstande von Pesticiden und anderen Fremdstoffen in Nahrungs- und Futtermitteln PDF

133 Pages·1969·6.87 MB·English
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RESIDUE REVIEWS VOLUME 28 RESIDUE REVIEWS Residues of Pesticides and Other Foreign Chemicals in Foods and Feeds RUCKSTANDS-BERICHTE Riickstande von Pesticiden und anderen Fremdstoffen in Nahrungs- und Futtermitteln Edited by FRANCIS A. GUNTHER Riverside, California ADVISORY BOARD F. BAil, Berlin, Germany· F. BRO-RAsMUSSEN, Copenhagen, Denmark J. W. COOK, Washington, D.C. • D. G. CROSBY, Davis, California S. DORMAL-VAN DEN BRUEL, Bruxelles, Belgium C. L. DUNN, Wilmington, Delaware • H. FREHSE, Leverkusen-Bayerwerk, Germany J. C. GAGE, Macclesfield, England· H. GEISSBUm.ER, Stein AG, Switzerland S. A. HALL, Beltsville, Maryland • T. H. HARRIS, Bethesda, Maryland L. W. HAZLETON, Falls Church, Virginia • H. HURTIG, Ottawa, Canada O. R. KLIMMER, Bonn, Germany • G. K. KOHN, Richmond, California H. F. LINSKENS, Nijmegen, The Netherlands· H. MAIER-BODE, Bonn, Germany N. N. MELNIKOV, Moscow, U.S.S.R. • R. MESTRES, Montpellier, France P. DE PIETRI-TONELLI, Milano, Italy· R. TRUHAUT, Paris, France VOLUME 28 SPRINGER-VERLAG BERLIN • HEIDELBERG • NEW YORK 1969 All rights reserved. No part of this book may be translated or reproduced in any form without written permission from Springer-Verlag. ISBN-13: 978-1-4615-8454-4 e-ISBN-13: 978-1-4615-8452-0 DOT: 10.1007/978-1-4615-8452-0 © 1969 by Springer-Verlag New York Inc. Softcover reprint ofthe hardcover 1s t edition 1969 Library of Congress Catalog Card Number 62-18595. The use of general descriptive names, trades names, trade marks, etc. in this publication, even if the former are not especially identified, is not to be taken as a sign that such names, as understood by the Trade Marks and Merchandise Marks Act, may accordingly be used freely by anyone. Title No. 6631 Preface That residues of pesticide and other "foreign" chemicals in food- stuffs are of concern to everyone everywhere is amply attested by the reception accorded previOUS volumes of "Residue Reviews" and by the gratifying enthusiasm, sincerity, and efforts shown by all the in- dividuals from whom manuscripts have been solicited. Despite much propaganda to the contrary, there can never be any serious question that pest-control chemicals and food-additive chemicals are essential to adequate food production, manufacture, marketing, and storage, yet without continuing surveillance and intelligent control some of those that persist in our foodstuffs could at times conceivably endanger the public health. Ensuring safety-in-use of these many chemicals is a dynamic challenge, for established ones are continually being dis- placed by newly developed ones more acceptable to food tech- nologists, pharmacologists, toxicologists, and changing pest-control requirements in progressive food-producing economies. These matters are of genuine concern to increasing numbers of governmental agencies and legislative bodies around the world, for some of these chemicals have resulted in a few mishaps from improper use. Adequate safety-in-use evaluations of any of these chemicals per- sisting into our foodstuffs are not simple matters, and they incorporate the considered judgments of many individuals highly trained in a variety of complex biological, chemical, food technolOgical, medical, pharmacological, and toxicological disciplines. It is hoped that "Residue Reviews" will- continue to serve as an integrating factor both in focusing attention upon those many residue matters requiring further attention and in collating for variously trained readers present knowledge in specific important areas of residue and related endeavors; no other single publication attempts to serve these broad purposes. The contents of this and previous volumes of "Residue Reviews" illustrate these objectives. Since manuscripts are published in the order in which they are received in final form, it may seem that some important aspects of residue analytical chemistry, biochemistry, human and animal medicine, legislation, pharmacology, physiology, regulation, and toxicology are being neglected; to the contrary, these apparent omissions are recognized, and some pertinent manuscripts are in preparation. However, the field is so large and the interests in it are so varied that the editor and the Advisory Board earnestly solicit suggestions of topics and authors to help make this international book- series even more useful and informative. "Residue Reviews" attempts to provide concise, critical reviews of timely advances, philosophy, and significant areas of accomplished or needed endeavor in the total field of residues of these chemicals in foods, in feeds, and in transformed food products. These reviews are either general or specific, but properly they may lie in the domains of analytical chemistry and its methodology, biochemistry, human and animal medicine, legislation, pharmacology, physiology, regulation, and toxicology; certain affairs in the realm of food technology con- cerned specifically with pesticide and other food-additive problems are also appropriate subject matter. The justification for the prepara- tion of any review for this book-series is that it deals with some aspect of the many real problems arising from the presence of residues of "foreign" chemicals in foodstuffs. Thus, manuscripts may encompass those matters, in any country, which are involved in allowing pesticide and other plant-protecting chemicals to be used safely in producing, storing, and shipping crops. Added plant or animal pest-control chem- icals or their metabolites that may persist into meat and other edible animal products (milk and milk products, eggs, etc.) are also residues and are within this scope. The so-called food additives (substances deliberately added to foods for flavor, odor, appearance, etc., as well as those inadvertently added during manufacture, packaging, distribu- tion, storage, etc.) are also considered suitable review material. Manuscripts are normally contributed by invitation, and may be in English, French, or German. Preliminary communication with the editor is necessary before volunteered reviews are submitted in manu- script form. Department of Entomology F.A.C. University of California Riverside, California May 28,1969 Table of Contents Insecticide residues in California citrus fruits and products By F. A. Gunther.................................... 1 Subject Index ............................................ 121 Manuscripts in Press ...................................... 128 Insecticide residues in California citrus fruits and products* By FRANCIS A. GUNTHER\)\) Contents I. Introduction ................................................. 2 II. Residue legislation ............................................ 6 III. Tolerances .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 a) Establishment of tolerances .................................. 7 b) Pertinent insecticide tolerances for citrus fruits .................. 9 IV. Generalized insecticide residue behavior on and in citrus fruits ....... , 14 a) Degradation and persistence curves ........................... 15 b) Established persistence curves ................................ 34 c) Residue half-life concept .................................... 34 d) Uses of half-lives and persistence curves ........................ 39 e) Effects of variety on residues ................................. 41 V. Insecticide residues in citrus products ............................. 42 a) Citrus juices .............................................. 42 b) Laboratory-prepared citrus pulp cattle feed ..................... 47 c) Citrus oils ................................................ 52 d) Orange marmalade ......................................... 57 e) Dried and candied orange rind ............................... 58 VI. Insecticide residue removal by washing ........................... 58 VII. Systemic insecticides as residues ................................. 59 VIII. Some market survey insecticide residue data ....................... 64 a) The French program ....................................... 64 b) The California-Arizona Citrus League program .................. 64 IX. Multiple residue methods for citrus fruits .......................... 69 X. Developmental citrus residue-analytical methodology with fresh fruits.. 74 a) Presampling considerations .................................. 74 b) Sampling procedure ........................................ 76 c) Storage of fresh samples ..................................... 78 d) Processing of samples ...................................... 79 e) Storage of extractives ....................................... 92 f) The analysis .............................................. 93 • Presented in partial and summary form at the International Citrus Sym- posium, 19 March 1968, Riverside, California: see GUNTHER and WESTLAKE (1968) in "References" section . •• Department of Entomology, University of California, Riverside. 1 2 F. A. GUNTHER XI. Miscellaneous aspects and conclusions ............................ 96 a) Current insecticide dosages in California ....................... 99 b) Adequate developmental, surveillance, and mOnitoring programs for pesticide residues ...................... 99 c) Insecticide metabolites and other alteration products in citrus fruits .. 101 d) Citrus insecticides in the grove environment ..................... 102 e) Deposition and persistence of insecticides on leaves versus fruits . . .. 106 Summary ......................................................... III Resume .......................................................... 112 Zusammenfassung .................................................. 113 References ........................................................ 114 I. Introduction Prior to about 1945 it was not realized that spray and dust deposits of most organic insecticidal l chemicals penetrated, in the field, into subsurface regions of sprayed citrus fruits, even though they were generally nonsystemic in action, as with some of the DN compounds and rotenone. Also, emphasis on «residues" (deposits) prior to this same time was on correlations with pest-control efficacy rather than on safe consumption of the treated commodity, so that initial deposits and aged deposits were most often obtained as weight of insecticide per unit areas of leaf (foliage) tissue 2 rather than on and in mature fruits, as with sulfur, lime-sulfur, and lead arsenate, because insect popula- tions were usually evaluated on leaves or twigs rather than on fruits. In connection with the field performance of DDT and other new in- secticides against insects and mites in citriculture, however, it was realized shortly after 1940 that the slow disappearance or attenuation from leaves of these (DDT) surface deposits and effective residues from organic pesticides signified at least partial penetration into subsurface tissues (GUNTHER 1946 and GUNTHER et al. 1946). It was also im- mediately recognized (BOYCE 1946) that pesticides penetrating into leaf tissues would probably also penetrate into fruit tissues, and that these penetrated residues in citrus fruits, for example, could conceiv- ably constitute a new type of hazard to the consuming public. Atten- tion was therefore turned immediately to fruits and other edible plant parts as the residue analytical substrates, and correlations of deposits and residues with biological performance became of secondary im- portance as the pharmacological and toxicological significance of per- sisting and altering «residues" was recognized. Because of laboratory 1 The term "insecticide" often includes those chemicals used for mite control, or "acaricides." Both types of pest-control agents are considered as insecticides in the present report. Only the organic insecticides are included. Chemical designa- tions of insecticides mentioned in text are listed in Table XXXII. 2 See section XI d) for a discussion of deposits and residues expressed as p.p.m. (weight basis) versus p,g./cm.2 (area basis). Insecticide residues in citrus fruits 3 convenience and presumed parity of public health significance, these values were now expressed on a part-per-million basis for all foodstuffs. Residue chemistry and biochemistry as known today around the world were therefore conceived within the citrus industry, and the first true surface and subsurface residue evaluations were made with mature lemons and oranges in the Department of Entomology, Univer- sity of Califomia Citrus Experiment Station, Riverside. The term "residue" was coined to refer to aged and usually penetrated pesticide chemicals and their in situ alteration products, particularly on and within the edible parts of treated plants and within animal tissues. Thus, "deposit" now refers to pesticide chemical initially laid down by the field treatment, whereas "residue" refers to material on and in the plant part after the processes of weathering, metabolism, hydrolysis, penetration, etc., have begun and on (e.g., wool) and in animal parts. Additionally, chemical so located as still to be available to the pest is known as an "effective deposit" or "effective residue" depending upon both its age and its major location with respect to the plant cuticle; this terminology does not apply to animal tissues (GUNTHER and BLINN 1955, GUNTHER 1962, 1966, and 1968 a). Federal legislation for control of food quality since 1954 [Public Law 83-518 et seq. and the Federal Insecticide, Fungicide, and Ro- denticide Act of 1947 et seq. (HARRIS and CUMMINGS 1964)] has dictated that tolerance assignments (legally permitted maximum amounts of residues) and classifications for pesticides on and in raw agricultural commodities shall be based in part upon particular formu- lations and particular dosages applied in the field, with specified tim- ing in relation to harvest or blossoming periods and to numbers and spacings of multiple applications if required. Acceptable residue in- formation and tolerance assignments are therefore commonly based upon extensive biological testing in the field with formulations thought at that time to be standardized and with dosages that would achieve the desired pest control. Subsequent significant changes in formula- tions and recommended dosages require reconsideration by the licens- ing and registration authorities, with probable reconsideration of tolerance assignment if dosages or frequencies of applications are increased or if minimum intervals to harvest are decreased. Residue information developed in achieving legal commercial use of a pesticide chemical is therefore felt to represent the maximum residues that could actually occur in agricultural commodities at har- vest 3 if the label instructions on the pesticide container were strictly and consistently followed. Consequently, for every pesticide in every use on every crop plant there exist often abundant data (usually un- published) illustrating maximum and average residues that will result from good agricultural practice. If dosages, timing, formulations, and 8 Ergo, from "good agricultural practice." 4 F.A.GUNTHER numbers of applications are not appreciably changed after legalized use is achieved, residues found in "market surveys," "market-basket studies," residue surveillance 4 programs, and residue monitoring II programs with a specific crop should reflect the original developmental data provided those original data were representative of the treated crop and straddled a harvest period rather than a specific harvest date, e.g., residues from 15 to 60 days after application versus exactly 30 days after application for mature citrus fruits. Should the pre- and post-tolerance-assignment residue data differ markedly - without changes in formulations, dosages, numbers of applications, or timing - the major causes to be suspect are changes in the residue analytical methodology or in the adequacy of the sampling for either the initial or the monitoring program. In general, residue analytical methodology is steadily improving in both quality and quantitative reliability and more incisive data would be expected today than were achievable 10 to 20 years ago, especially in terms of prob- able metabolites included in the "apparent" residue value; on the other hand, developmental residue data are usually obtained from extrava- gantly large field samples and number of replicates to represent the crop in the field, whereas monitoring and other quality-assurance data are often from statistically meager samples taken somewhere between field and consumer, often at the end of the packing house line with citrus fruits. In some important instances, earlier and current analytical procedures can be compared for reliability, but it is not easily possible to correlate a field sampling program with the usual market sampling program; the former presumably establishes a range of values en- compassing the mean or average residue load from the field applica- tion, whereas the latter ideally should demonstrate the maximum residue present in a shipment, a carload, a lot,a carton, etc. Some guidelines for field-sampling programs have been adequately estab- lished for various crops; how to sample in a postharvest residue sur- veillance or monitoring program is still a matter of empirical judgment influenced in part by the time available to the sampler, but mostly by the economics of purchasing the samples, the nature and size of the crop unit on the market, the size of the lot involved, sample storage space available to the residue laboratory, the grinding and extraction equipment available in the laboratory, and others. Over a long enough period, the continuing "market-basket survey" initiated by the U.S. Food and Drug Administration is undoubtedly the most realistic ap- proach to this problem. As has been shown (DE Vos 1968), taking half a dozen fruits from a carton or market display is not a realistic answer 4 Examining in a suspect area or situation, usually in the field but often in the wholesale market; guided samples. II Examining at random, usually with market or wholesale samples; random samples.

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