Anal. Chem. 1985, 57, 1 R-15R
Pesticides Joseph Sherma* Chemistry Department, Lafayette College, Easton, Pennsylvania 18042
Gunter Zweig Office of Pesticide Programs, US.Environmental Protection Agency, Washington, D.C. 20460
This review on the analysis of pesticides covers the period of December 1981to December 1984. Again, we relied heavily on the excellent coverage in the two main abstracting journals, Chemical Abstracts and Analytical Abstracts. We also covered the main repository of information on pesticide analyses, Journal of the Official Association of Analytical Chemists (J.Assoc. Off. Anal. Chem.) and the Journal of Agricultural and Food Chemistry (J.Agric. Food Chem.). Although there seemed to be no dramatic breakthrough to report, the following analytical techniques appeared to have made significant advances in the analysis of pesticides: capillary gas chromatography (GC); GC coupled with mass spectrometry (MS) for the identification of pesticide residues, metabolites, and contaminants (e. dioxins); high-performance liquid chromatography (HPL& with reversed and other bonded phases and electrochemical detectors; high-performance thin-layer chromatography (HPTLC) and quantitation by automated densitometry. Although an occasional report on paper chromatography, usually from a developing nation, may be found in the international literature, TLC has mostly displaced the older technique, paper chromatography. A few reports on the use of immunoassay for pesticide analysis of specific compounds have appeared in the literature and are reported in this article. As we have observed in previous reviews, the sensitivity of most methods has not gone beyond the picogram level, although capillary GC-electron capture (EC) is capable of detecting femtogram quantities. We emphasize again, that many r e p o in ~ the literature devote much space to cleanup procedures and sample preparation. The rule seems to persist that a clean sample gives the best results! This review is devoted mostly to the analysis of pesticide residues and standards but not pesticide formulations. Compounds which in themselves cannot be classified as esticides, but nevertheless exhibit similar chromatographic l&ehavior,are covered in this chapter and include polychlorinated biphenyls (PCBs), phthalate esters, chlorinated dibenzodioxins, and furans. We found many reports on the analyses in a variety of matrices of organochlorine, organophosphorus, carbamate, and synthetic pyrethroid pesticides. As in previous years, the first part of the review deals with general topics of pesticide analysis, followed by the coverage of specific classes of pesticides. For the sake of clarity, we have broken down the references according to specific topics, while endeavoring to cite papers from readily available journals, or if important enough and reported in more obscure journals, we have also given the corresponding citation from the abstract journal. GENERAL Basic principles and practices for the analysis of pesticides (6A), as well as improved cost-effective approaches to residue analysis (I3A), have been discussed in two recent publications. Chromatographic techniques for the analysis of hazardous impurities in pesticides have been described (3A). Collaborative studies help to control the systematic error of analytical methods (IIA), like GC (8A). Simplified methods for the quantitative analysis of pesticide residues have been summarized (24A). The behavior of pesticides in the aquatic environment (23A) and the analysis of pesticide residues in an agricultural settin have been reviewed (I4A, 22A). The separation ancf purification of pesticide metabolites (17A) and their identification by soft ionization MS technique (IOA) have been the subject of two papers. The nature, identity, and properties of nonextractable soil and plant 0003-2700/85/0357-1R$06.50/0
pesticide residues have been discussed (12A), raising the important problem of their analyses and the challenge to the pesticide analytical chemist. Advances in pesticide residue analysis in food have been reviewed in two recent publications (20A, 25A). The application of MS in the regulatory analysis of pesticides and industrial chemicals in food and feed commodities has been reviewed (4A),and HPLC has been compared with GC in food analysis (21A). Residue methods for the analysis of contaminants, among them pesticides, in milk and milk products have been reviewed (2A). Rapid screening methods for pesticide residues and mycotoxins in food have been discussed in a recent paper (7A). A number of review papers have dealt with the analysis of aromatic amines (9A), organochlorine compounds (9A, 15A), polychlorinated dioxins and furans (18A), and carbamates (IA, 19A). An empirical pattern-recognition scheme has been proposed for the interpretation of chromatograms of complex mixtures, provided that the experimental results are highly reproducible (16A).
BOOKS AND REVIEWS A number of recent books or new editions of previously published books on the chemistry of pesticides have appeared during this period: the second edition of a book on organic plant protective agents and pesticides (1OB);the third edition of the International Pesticide Directory (12B); on the metabolism and mode of action of pesticides (8B);Vol. 2 of the Pesticide Analytical Manual by the Food and Drug Administration (7B) which continues to be an invaluable guide to the pesticide analyst; the 7th edition of Pharmacological and Chemical Synonyms (13B); Volume 3 of CIPAC methods for pesticide formulation analyses, containing the latest methods for pesticides distributed internationally (9B). A number of useful review articles covering the analytical methods and chemistry of pesticides are recommended reference material for the practicing pesticide chemist: chromatography of pesticides (6B);analytical methods for drugs, pesticides, and industrial chemicals (4B); bound pesticide residues in soil and plants (11B); pesticides in food (21B). Several books which have been published during this reporting period are on the topic of environmental chemistry, including pesticides (lB, 14B). A three-volume treatise on the analysis of pesticides in water, published recently, covers the literature through 1977 (3B). The 8th edition of Approved Methods by the American Association of Cereal Chemists might be useful for the chemist wishing to analyze fumigant residues in cereals (2B). Specific classes of pesticides have been covered in recent books and reviews: the metabolism and analysis of pyrethrins and pyrethroid insecticides ( 1 7B, 23B); the chemistry of orchlorinated dioxins (18B); ganophosphorus pesticides (5B); the metabolism of fungicides (19B); 5th edition of the useful Herbicide Handbook (20B); and a series of review articles on the triazine, substituted urea, and phenoxyalkyl acid herbicides (16B, I5B, 3B). SAMPLING AND CLEANUP General. Quality control by collaborative studies remains an important endeavor in order to establish the ultimate accuracy of samples for pesticide analyses performed in different laboratories (40C, 46C, 47C). An interlaboratory study has been performed to validate an official EPA method for base/neutral, acid, and pesticide priority pollutants (38C). Directions are recommended to establish maximum pesticide 0 1985 American Chemical Society
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residue limits in crops (41C). General approaches for the identification of pesticide residues in foods of unknown origin were reviewed (37C). The stability of standard solutions of pesticides under different storage conditions was studied, and caution must be exercised in the case of several pesticides which degrade at ambient temperatures and are affected by light (15C). Analytical problems in the commercial development of plant protective agents (pesticides) have been reviewed (18C). Synthetic nitro musk fragrances have been shown to be potential contaminants using the recommended AOAC-multiresidue methods for cleanup and GC analysis ( 5 2 0 Research on automatic cleanup of samples prior to pesticide analysis continues and may eventually lead to commercial instrumentation (13C, 14C, 17C). Sample preparation for organic trace analysis, including that of pesticides, has been reviewed leading to recommendations for the practicing analyst ( 2 0 . The adsorptive properties of Tenax for the preconcentration of chlorinated pesticides from water and air has been investigated and found useful (IC). Gel permeation chromatography on Bio Beads SX-3 proved to be a universal cleanup method for many pesticides from fruits and vegetables (11C). Using macroporous organic sorbents (e.g., Separon SE) for the cleanup of phenoxy herbicides from water might result in high “blank” values in subsequent analyses due to trapping of analytes (36C). The chromatographic behavior of several classes of esticides (carbamates, phenylureas, etc.) has been studied gy HPLC with a silica gel column and a ternary mobile solvent system ( 3 5 0 Steam distillation for many pesticides, except toxaphene and methoxychlor, has resulted in better than 75% recovery from soil and plant tissues (32C). A patented micro cleanup and concentration apparatus consists of an LC column and filament concentrator (42C). A rapid procedure has been described for the extraction of pesticide residues from fabric
W).
Cleanup of Environmental Samples. The US. Geological Survey has conducted a pilot study to investigate if ita water reference standard program for inorganic constituent can be expanded to include pesticides (1OC). The use of Amberlite XAD resins for aminocarb and metabolites from water, followed by GC, has been found to result in high extraction efficiency (23C). Preconcentration of organophos horus (19C) and chlorinated (4C) pesticides from water c o u d be achieved by the adsorption on graphitized carbon black. Pesticide Sam les from air have been concentrated on several resins: mberlite XAD for chlorinated, including fumigants (3C, 51 C); Tenax-GC for chlorinated (3C) and fenitrothion and aminocarb (21C); XE-340 for chlorinated ( 5 0 0 ; silanized silica gel for chlorinated ( 4 5 0 Phosphine methods have been evaluated with seven types of detector tubes (22C). Although methanol and acetone were found to be the most frequently used solvents for the extraction of pesticides from soil, a theoretical approach based on the known molecular properties of solvents and compounds should lead to a more efficient process (6C). Two methods for the isolation of “dislodgeable” foliar residues of sulprofos, permethrin, and methomyl were compared, and the method which does not use a surfactant is preferred as being the more rapid one (48C). Isolation from Fats and Oil. The analysis of PCB’s in industrial oils has been studied and recommended procedures were developed (43C). Sweep-codistillation cleanup procedures for organochlorine pesticide residues, PCB’s, and pentachlorophenol from animal fat have been described (26,33C). Less volatile pesticides (carbaryl, parathion, and aldrin) have been isolated from fat using a simultaneous steam distillation and extraction apparatus ( 9 0 Different methods for the isolation of pesticides from fat and lipids have been the subject of further refinement and innovation: PCB’s in fish (3OC);.lipophilicorganochlorine pesticides in fat (39C); gel permeatlon chromatography (29C); for milk and oil seeds (27C); the optimization of alumina adsorbent (12C). Nonfatty Products. The multiresidue method for pesticides in nonfatty foods has been further improved (28c). The multiresidue method has been successfullyapplied to the analysis of quinomethioate in apples and oranges (20C). The same method has been applied to the analysis of pesticide residues in kiwifruit, apples and berries. (160. The extraction
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ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985
efficiency of various solvents for pesticide residues in plants demonstrated that methanol was generally the most effective solvent (49C). Method for the analysis of residues of organophosphorus compounds (OP compounds), ethylenebiddithiocarbamates) (EBDC), Fusarium toxins, and total Br in barley, malt, and hops have been developed (44C). Specific Compounds. Water samples containing chlorophenols (not pesticides in the strictest sense) have been enriched prior to GC/MS on Sep-PAK CISreversed-phase adsorbents (34C) and on XAD resin and activated carbon (5C). Steam distillation for the recovery of phenols from soil has been evaluated (31C). Two adsorbents, XAD-2 and Florisil, have been evaluated and found highly efficient for the sampling of 2,3,7,8-tetrachlorodibenzodioxin (TCDD) (7C). Abscisic acid and indolyl-3-acetic acid have been separated by a three-phase extraction and dialysis technique (25C); another purification method for abscisic acid involved an initial extraction with buffered (pH 8) methanol and then hexane, extraction into ether at pH 3, and final purification on Sep-PAK CIS(24C). GAS CHROMATOGRAPHY (GC) Capillary GC. The advanta es of capillary vs. packedcolumn gas chromatography is t[e increased resolution and shorter analysis time (500). Comparison of retention ratio data for pesticides separated on packed columns and capillary columns has been made (150). Relative retention times of 194 pesticides have been determined on a 15-m long capillary SE-30 column (350). Sample preparation of biological and environmental samples for capillary GC has been reviewed (330). Pesticide residues in foods which were difficult to analyze by packed-column GC were determined by capillary GC using a split/splitless inlet system and electron capture (EC) detector (120). Multidetection of pesticides analyzed by capillary GC was achieved by parallel N- and S-specific detectors (130). Using two capillary GC columns in parallel was found to be suitable for the analysis of PCB’s and chlorinated pesticides found in the same sample (380). Similarly, combining two capillary columns and connecting them to a selective flame photometric detector and EC detector, the authors screened over 100 halogenated and OP-pesticides (440). On-column injection of samples analyzed by capillary GC-, combined with MS gave higher sample transfer and greater sensitivity than the splitless injection system (470). Other applications and innovations involving capillary GC which have been used for pesticide analysis are as follows: capillary GC/MS computer identification of pesticide metabolites and confirmation of pesticide residues (180); fused silica on-column injection of chlorinated pesticides with an ultra-lowvolume rotary valve (190); automated pesticide residue analyses of food by fused-silica capillary column GC (160, 430); 50-hm (i-d.) capillary GC for fast GC of chlorinated pesticides detected by EC (390); the use of a polar glass capillary column using polyethylene glycol adipate as stationary phase for a large number of pesticides (340). Specific examples of the application of capillary GC which have been reported are as follows: toxaphene, identified by electron impact chemical ionization (C.I.) MS (370); ethylenethiourea and propylenethiourea in hops, beer, and grapes (320); separation of PCB’s and EPA’s non-priority pollutants on wall-coated fused-silica open tubular columns (290,200). Retention indexes for chlorinated benzenes and biphenyls have been determined for programmed temperature capillary column GC (310). A useful technique for the automated development of an optimum temperature program for capillary GC has been reported (420). Detectors for GC. Selective detection for haloforms and herbicides in water has been discussed, including EC, MS (sin le ion), and flame photometric detectors (60). Further mocfification of the Hall electrolytic conductivity detector (140) and an interlaboratory study of the Hall detector for halogen-containingcompounds (PCB and pesticides) has been completed (90). False positive halogen responses by the Hall detedor of eggplant extracts were found to be long-chain fatty acids (70). During the ast 2 years, several new GC detectors have been developed a n i evaluated: a high-temperature DC EC (400); a detector made of boron nitride which can be used alternatively in the photoionization and electron capture modes
PESTICIDES
ticidea (270)Mixed-bed . OJlUmns contain'
two silicones
K",been found to be superior to sin le p a c a columns for
the analysis of pesticides in food (IODf i d fumigant residua 1 n gain .(110). hlonnated bydroearbons and phenols have been analyzed by GC on polar columns (25D); hexachlorocyclohexane(HCH) isomers and metabolites (phenols) from aqueous media have been isolated and analyzed by GC (240). The multiresidue GC method for organochlorine compounds in poultry fat has undergone collaborative studies (ZD). A thorough, statistical evaluation has been completed on the GC analysis of PCBs in industrial oils (21D).
bbchembtry hom tha UnlversHy of Maryland. He has wlds sxpdencs in blochem& by and c h a m a t ~ a p h vOf p*l!€ldes and has puM(shed many research ankles and W s in me areas of hls s p c l a l ~ .
(230);a microvolume EC detector suitable for capillary GC (49D); an indium-sensitized flame photometric detector for CI cpmpoyds (48D);a tunable selective thermionic detector to differentiate unambiguously between N and P compounds (460). Other developments in detector technique are a power-modulated microwave-induced plasma detector with enhanced sensitivityfor capillary GC for CI and Br compounds with a 10' discrimination with respect to C (SD),a rapid scanning plasma emission detector for multielement quantification of halogenated pesticides and other compounds W D ) ,an oxygen-doped ion-mobility detector for enhanced response to CI compounds ( 3 0 ) ,and GC coupled to infrared Fourier-transform spectroscopy for the identification of mirex and related compounds (22D). A computer program in BASIC has been written to combine data from an EC and a flame photometric detector (410). GC/Mass Spectrometry. GC coupled to MS continues to he a favored techniaue for the absolute identification of pesticide residues and metabolites as attested by a number of recent publications: negative ion C. I. MS (450); the evaluation of an automatic method for the detection of chlorinated pesticides by a cornhination of GC/MS under the control of an DS55 data system (36D).Positive and negative ion data, simultaneously obtained under C. I. conditions, and coupled with a fused silica capillary GC-column, has been found useful in the identification of pesticides which are on the list of EPA priority pollutants (5D). The confidence limits for the detection of 2,3,7,8-TCDD by isotope dilution GC MS have been discussed in a recent review (28D). A new C/MS methodology has been found to he suitable for the analysis of insect pheromones (170). Procymidone from imported f d s has been resolved by packed column GC and suhse uently identified by MS (4D). Water samples containing heaicides have been enriched on ass e through a Carbotrap and analyzed after desorption y G /MS (260). Miscellaneous Studies with GC. Insect pheromones in nanogram quantities have been identified by pre aring characteristic derivatives after initial GC, followed y! the separation of the derivatives by GC (ID). The herbicide lyphosate has been analyzed by GC as the dimethyl-tert%utylsilylderivative (300). A method designed for the anal sis of air pollutanta in a factory setting by the use of grapzitized-black adsorbenta, followed by GC of the desorbed compounds. might find a p plication in the analysis of fumigants and other airborne
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HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC) Detectors and Columns. HPLC continues to find a useful place aa an analytid tool for the separation and determination of pesticide residues. One of the shortcomings of this technique has been the lack of specific detectors, so that the few reporb of new HPLC detectors applicable to pesticide analysis are doubly welcome. The commercially available photoconductivity detector has been evaluated for a number of pesticides below ppm (2IE)and has been applied to the analysis in fruits and vegetables of the fungicides captan, folpet, and captafol at the ppb level (22E).Thirty-five pesticides and metabolites have been successfullyanalyzed by HPLC using a fluorescence detector (13E). Quenched and sensitized phosphorescence of polychlorinated naphthalenes and biphenyls has been utilized for the detection of these com ounds separated hy liquid chromatography (IOE). RadiolaLled "C organochlorine pesticidea have been simultaneously detected after HPLC with a UV detector and a radioactivity flow detector (160. An impmved interface between a liquid chromatograph and an electron capture detector promises to offer specific detection capability for organochlorine compounds (6E). Organothiophosphate insecticides have been detected after HPLC hy on-line photo1 sis and electrochemical detection (SEI. Jignificant advances have been made on interfacing HPLC with MS and applying this technique to pesticide problem: a report on the modification of the Vespl desolvation chamber on a Finnigan 4500 MS (I9E); the design of a gas-nebulized direct liquid introduction interface (IO;a postcolumn buffer addition for the thermospray device suitable for HPLC and MS spectra of carbamate and urea herbicides W E ) ; the comhination micro-HPLC and MS for on-line analysis of phenylurea herbicides (24E). A special Pt-packed short precolumn connected to a Clereversed column was capable of separating aniline from phenylurea herbicides in water ( I I E ) . Phenols and substituted henols resent in water were fmt pasaed through cyclobexyl E ndeco ! ase column, eluted with methanol, and separated by HPLC on Sepralyte C8 (7E). Several reversed-phase columns have been evaluated for the analysis of plant hormones ( I S E ) . Parathion and metabolites in h l d serum have been directly analyzed by injecting serum samples on to a microcolumn, LiChrosorh RP-8 and using water or aqueous methanol as mobile phases (24E). Applications. HPLC haa found wide use for the solution of numerous pesticide analytical problem. HPLC of pesticide residues in environmental samples has been reviewed (4E). Retention data of 560 drugs and insecticides from reversedphase HPLC have been published (5E). Airborne pesticides, after concentration on Tenax and desorption, were analyzed by HPLC and detected by W or electrochemid detector (for phenols) @E). Oxamyl and ita oximino metabolite have been analyzed by HPLC on a Zorhax ODS column after cleanup through a Sep-PAK (17E).A simplified HPLC method for glyphosate in fruits and vegetables has been developed and is based on postcolumn fluorogenic labeling (15E). Dithiocarbamates have been analyzed by HPLC on two different types of bonded phases and by the interaction of tetraalkylammonium salts (IZE). The experimental insecticide, nifluridide, from water has been analyzed hy HPLC on a LiChrasorh RP-I8 reversed-phase column after concentration on a Sep-PAK CIScartridge (23E). EPAs priority pollutants have been analyzed by HPLC on ODs-bonded phases (SO. HPLC has been used to calculate quantitative structure-activity relationships for herbicides based on the hydrophobicity of these compounds (3E). ANALYTICAL CHEMISTRY. VOL. 57. NO. 5, APRIL 1985
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THIN-LAYER CHROMATOGRAPHY (TLC) Although most advances in pesticide analysis have taken place during the past 2 to 4 years in the fields of GC and HPLC, thin-layer chromatography (TLC) has retained its status as a valid and simple method for qualitative and, in the view of some, even quantitative method of analysis for pesticide residues and metabolites. It appears that many papers on this subject originate from researchers in less developed countries, which is plausible due to the lack of sophisticated instrumentation and the shortage of repair facilities in these countries. A review paper on the application of two-dimensional TLC to the analysis of environmental pollutants, inorganics, and pesticides covers the literature through early 1982 ( 2 2 9 . A novel technique for the analysis of organophosphate (OP) insecticides and their metabolites combines TLC and MS without the elution of substances from polyamide-TL plate by the direct introduction of the separated substances into the ion source of the MS (2F). Several papers report on the TLC of acetylcholinesterase-inhibitinginsecticides, as follows: OP compounds are visualized on the plates with cholinesterbe reagent and a suitable substrate, e.g., indoxyl acetate or acetylthiocholine (13F), and quantified by reflectance scanning; screening for OP and organochlorine compounds in animal tissues (1OF); OP compounds in vegetables (11F);OP and carbamates in fruit and vegetables (21F);and OP residues in toxicological investigations (20F). Several carbamates have been separated on thin layers of silica gel coated with 1% zinc acetate (16F). A newly developed spray reagent for organochlorine compounds on TL is 3,3’,5,5’-tetramethylbenzidineat a detection limit of 0.2 pg (SF). Thionophosphoric esters and decomposition products can be visualized and semiquantified with the 12-azidereagent (IF). Herbicides which inhibit the Hill reaction (photosynthesis) can be visualized on TLC plates by a spray of chloro last homogenate and 2,6-dichloroindophenol and exposure o?the plates to white light (7F). The resolving power of solvents for TLC of triazines was found to be related to the lipophilicity of the solvent (6F).A structure and TLC mobility relationship for tebuthiuron and related compounds has been established (15F). Indole-3-aceticacid decomposes rapidly on silica gel plates, and caution must be exercised when using this chromatographic technique for IAA (SF). Direct reflectance densitometry and decrease in fluorescence were used for TLC of herbicides on silica-gel layers precoated with a fluorescence indicator (4F). Organic acids have been separated on TLC using CaSO, plates; this technique may be suitable for acid pesticides (3F). High-performance TLC (HPTLC) has been used for the analysis of organotin compounds (SF). According to the authors (18F),they have been able to analyze toxaphene uantitatively by using a commercial extinction registering levice with integrator. Paraquat in toxicological investigations has been determined by TLC on silica-gel lates and visualized with Dragendorffs reagent (19F). A fielftest has been developed for the analysis of PCB’s by TLC and a quantitative evaluation by densitometry later in the laboratory (17F). Biphenyl residues in citrus and urea, carbamate, and anilide herbicides have been analyzed quantitatively by TLC and densitometry (14F,12F). MISCELLANEOUS TECHNIQUES Analytical techniques for pesticides are not exclusively based on chromatographic methods. This section is a review of other significant methods which have been described in the literature during this reporting period. A commercial automatic analyzer, Automatic Modules for Industrial Control Analysis (AMICA), produced in Switzerland, has been tested for the analysis of herbicides (1G);the unit consists of a liquid processor, a spectrophotometer, and an autosampler. A method is described for the calculation of pesticide partition between sediment and water at levels below the sensitivity of most methods (8G). Fluorine-containing pesticides have been analyzed by fluorine-19 Fourier transform NMR (17G). Toxic contaminants of technical-grade organo hosphorus insecticides have NMR 79G). Triple auadruDole mass been determined with 31P spectrometry has been applied to the andysk at f6mtogram levels of TCDD (20G). 4R
ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985
A number of pesticides have been examined on paper support surfaces for room temperature phosphorescence, which, it is claimed, mi ht be a suitable method for quantitative analysis (22G). Jimilar results were observed by the enhancement of luminescence of certain pesticides by the utilization of heavy atoms (13G). A bioluminescence assay for some aldeh de-containing insect pheromones utilizes the luciferase-catd zed oxidation of long-chain aldehydes in the presence of reiuced FMN (18G). The sulfur-containing insecticides methomyl and aldicarb and others containing nitro groups have been analyzed by differential pulsed voltammetry (polarography) (21G, 2G). Trichlorobiphenyl has been analyzed by adsorptive stripping voltammetry (15G). Capillary isotachophoresis has been utilized to quantify the level of asulam in soil (IIG). For the analysis of PCBs in the field, portable monitors have been developed, based on the principles of photoionization and IR spectroscopy (4G). Several analytical techniques recently reported are based on biological principles and reactions. For example, OP compounds in an aquatic environment were analyzed by an acetylcholinesterase assay using tritiated acetylcholine and extracting the released [SH]aceticacid with an organic solvent (IOG). Immunoassay continues to interest a number of investigators as to its applicability to pesticide analysis: 2,4-D by radioimmunoassay (14G);diclofop-methylby enzyme- and fluoroimmunoassay (19G);abscisic acid by a combination HPLC and radioimmunoassay (12G). Two reports on the use of immobilized cholinesterase electrodes demonstrate the feasibility of this technique in the analysis of OP and carbamate insecticides in the aquatic environment (7G, 16G). By use of an enzyme preparation of aryl hydrocarbon hydroxylase, it was possible to screen for compounds like dioxins, dibenzofurans, and PCB’s, which are known enzyme inducers (6G). By use of the organism Chlorella sorokiniana, a bioassay for atragine residues in soil was developed (5G). Most pesticide analysts are reluctant to reuse spent solvents in the extraction of pesticide residues from crops and other matrice$. A modified condenser has now been developed with which it was possible to reconstitute solvents, which when reused, showed no appreciable differences in results compared with those from fresh solvents (3G). CHLORINATED PESTICIDES General. The separation of chlorinated pesticides on columns of silica gel of varying degrees of porosity has been investigated (12H). Studies have shown that freezing of plant samples from the time of collection until final analysis assures optimum recovery (14H). In order to account for the interference of PCBs in the GC of DDT and related compounds in marine samples, chromatograms from an in-line KOH microreactor and a regular GC column are compared by means of a microprocessor (6H).Chlorinated pesticides have been determined in urine by neutron activation analysis (33H). Analysis of Human and Anihal Tissues and Fluids. Analytical methods and results for chlorinated pesticides in human milk continue to be reported (SH,32H, 41H). Modified cleanup methods for the GC of chlorinated pesticides in bovine milk have been developed (IH, 39H, 43H). Chlorinated compounds and phenols in tissues and body fluids of the rat have been analyzed by capillary GC (38H). GC methods have been used to determine organochlorine compounds in human liver samples (24H) and semen (40H, 44H). Twenty-one oranic industrial chemicals and pesticides were added to human %lood and extracts analyzed by GC; recoveries for hexachlorocyclopentadiene, mirex, and trans-nonachlor were unsatisfactory (4H). A collaborative study has been completed on a rapid GC-screening procedure for pesticides and PCB’s in fish (15H). Organochlorine pesticides, PCBs, and volatile halogenated hydrocarbons in fish from the upper Rhine and Lake Constance were analyzed by GC (2H). Environmental Samples. Organochlorine compodnds in wastewater were analyzed by capillary GC/MS (18H). Organochlorine compounds in river sediment were determined by capillary GC (45H). Chlorophenols in aqueous model solutions have been separated on TLC (42H). Analysis of Foods and Feeds. A simple fingerprinting technique for screening organochlorine residues in foods consists of pressing cut vegetables against o-tolidine-im-
PESTICIDES
column support material (141); optimum conditions for the separation of disulfoton, phorate, oxydemeton-methyl, and 0. their toxic metabolites (341);the determination of thioethers
re nated aper and exposing the paper to sunli ht, and if An b D b or H 8 H is present, instant colors develop official method for the preparation of feed samples for GC analysis has been reported (7H). Multiresidue analysis of organochlorine, organophosphorus, and synthetic pyrethroid pesticides in grain has been performed by GC and HPLC (323. Sample preparation of oil seeds and ve etable oil refinery byproducts, prior to pesticide analysis, has%een reported (37H, 47H). Pentachlorophenol. The widespread use of pentachlorophenol as a wood preservative and the possible health concern due to possible exposure have led to the development of a number of analytical methods and studies: the analysis of PCP in hardwood chips as the acetate by GC (17H);GC of the meth 1ester of the formulation and extract from treated ; of the methyl ester on QF-1 stationary timber (5danalysis phase or neopentyl glycol succinate (plus H3P04)for direct determination (28H); a simple spectrophotometric determination for water samples (1IH);the determination of pentachlorophenol in workers’ urine by HPLC after hydrolysis (13H) and in drinking water and urine by HPLC and electrochemical detection ( 3 0 ; and finally, the detection and determination in cultivated mushrooms as the methyl ester by GC (31H). Speoific Pesticides. The effect of water concentration in various organic solvents on the extractibility of dieldrin and methomyl residues has been investi ated (46H). ChIordane components in fish have been idended by capillary GC/MS (36H). Aldrin and dieldrin in soil were determined by mass fragmentography using heptachlor epoxide as internal standard (25H). Aldrin and endrin have been analyzed in sewage sludge by gas-liquid chromatography (GLC) (19H). The environmentalanalysis of toxaphene has been reviewed, and it was concluded that capillary GC with e3Ni electron capture detection in conjunction with MS is a suitabIe method (3423.Another approach to the analysis of toxaphene in water was taken by selecting and measuring representative peaks from a GC chromatogram and preparing individual calibration curves against “concentration of toxaphene” (26H). Toxaphene and chlordane in fish samples were determined by capillary GC coupled to negative chemical ionization (CI) MS (2.w. Two studies have been reported in which PCB congeners, mirex, and other organochlorine compounds were chromatoraphed by GC (9H, 2023. Trichlorodiphenyl sulfones have een shown to be a possible source of error in the determination of impurities in tetradifon, because the sulfones have the same molecular wei ht as 2,3,7,8-TCDD, a possible impurity of tetradifon (27Hf. A rapid GC method for haloforms, PCBs, and chlorinated pesticides has been developed (3523. Tetrachloronitrobenzene (TCNB) in potataes was analyzed by reversed-phase HPLC (1023. Concentrations of the insect-proofing agent, polychloro-2-(chloromethylsulfonamido)diphenyl ether on wool textiles and in textile liquors have been determined by normal bonded phase HPLC f29H). Reversed-phase ion-pair HPLC has been used to determine residues of the rodenticide chlorophacinone in animal tissues (21H). Chlordimeform and its metabolites have been determined in rice and husk on a DEGS GC column (1623.
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ORGANOPHOSPHORUS PESTICIDES General. Two methods have been compared for the analysis of azinphos-methyl, anticholinesterase (in vitro) and HPLC; it was found that the enzymic method was faster but that several metabolites could be assayed by HPLC simultaneously (221). Another comparison was effected between GC/MS and HPLC/MS for the analysis of another OP comanalogue; the conclusion was pound, coumaphos and its (0) that LC MS interface is more efficient (361). A study was reporte on the use of HPLC for the analysis of parathion, chlorpyrifos, and chlorpyrifos-methyl from rat tissues (331). A field method has been developed which will indicate above-tolerance residues of parathion on citrus fruit (281). Urinary metabolites of OP insecticide, dialkyl phosphorodithioates, can be extracted with great efficiency from aqueous medium by the equimolar addition of tetraphenylarsonium cation (101). Several studies have been reported on optimum conditions for the analysis of OP compounds by GC: the effect of column temperature (131); the effect of sample concentration and
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as their sulfone (81). Enzymic inhibition assay using cholinesterase (ChE) continues to be subject of studies: the quantitation of fenitrothion on TLC using ChE inhibition as visualization agent on TLC plates (see also ref 13F) (41). A study of enzyme sources for improved sensitivity of the in vitro methods showed that porcine liver had the highest Michaelis-Menten constant for fenitrothion (31). TLC methods have been applied to the analysis of the (0) analogues of fenthion, disulfoton, and phorate (261) and imidan (171). Mass spectrometry has been successfully applied to the identificationof OP compounds and their metabolites: CI-MS for the identification of isofenphos and its metabolites (51); negative CI (311);E1 fragmentation pattern of methamidophos by the use of stable isotopes ( W ) (351). Applications, Lipids from unpolished rice have been removed by precipitation with zinc sulfate, and after further cleanup, the final extract was analyzed by GC, using a flame photometric detector (11). The majority of reports on the analyses of OP compounds in crops and vegetables involve GC as the determinative step: OP sulfides, sulfoxides, and sulfones in fruit and vegetables (161); final identification of prothiophos in cabbage by MS (291); acephate, dimethoate, methamidophos, and omethoate in nectar (90. 14C-phoratefrom root crops (301) and pyrazophos (271) in plant products were separated by TLC, and the latter determined s ectrophotometrically (fluorescence) after elution. A modifiecfclean-upmethod for oxydemeton-methylresidues in cauliflower has been recommended (181). Due to the water solubility of most OP metabolites, methods for the analyses of these compounds in blood and urine continue to be refined: p-nitrophenol glucuronide and sulfate in blood and urine by enzymic hydrolysis and HPLC analysis (241, 251); disulfoton in urine and blood by GC MS (151); aminoparathion in postmortem specimens by C (61); N methylcarbamates and OP compounds in urine by GC (111). Acephate residues in water have been determined by HPLC on an RP-C8 column with aqueous methanol as mobile phase (21). Methods for the analysis of OP compounds and metabolites in milk have received wide attention: coumaphos by HPLC and confirmation by capillary GC/MS (191);GC determination of fenchlorphos, chlorpyriphos, coumaphos, and phoxim (231); OP residues by GC and a flame photometric detector (321). Residues of the defoliant DEF have been determined in water and fish tissue by GC (201); methods for OP residues in drinking water have received tentative approval by the use of GC, EC, or flame photometric detectors and one of the following column packings: SE-30, Apiezon L, DC-200, butanediol succinate, or OV-210 (71). A method is presented for the analysis of terbuphos in air by first adsorbing on charcoal tubes and after elution by GC (211).
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CARBAMATE PESTICIDES General Procedures. Cleanup of bovine rumen content extracts by solvent partitioning, sweep codistillation, and cellulose-carbon column chromatography was used prior to reversed-phase TLC of carbamate pesticides (194. Fourteen carbamate, urea, and thiocarbamate pesticides were determined in air by collection on filter paper, silica gel, or glass wool, followed by TLC or GC ( 2 4 . N-Methylcarbamate methoxy derivatives were prepared on-column by reaction of injected pesticides with trimethylanilinium hydroxide (354. Seven carbamate insecticides were determined at 5 to 50 ppb levels on fruits and vegetables by ethyl acetate extraction, C18-Sep-PAKcleanup, capillary GC, and thermionic detection ( 4 3 4 . A carbamate insecticide multiresidue method for fruits and vegetables involvin methanol extraction and cleanup by solvent partitioning and charcoal-Celite column chromatography was extended for the determination of additional pesticide types by RP-HPLC with fluorescence detection and GC with EC and FPD detectors (284. Carbamate pesticides were determined in water and soil by HPLC on a Cl8 column with detection limits ranging from 0.2 ng for methomyl to 10 mg for MTMC (144. Thermally labile carbamates and methylureas were determined by diANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985
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rectly coupled silica gel HPLC/MS with a movin -belt interface (65). Oxime carbamates were determinecf in environmental waters at 0.5-200 ppm concentration by extraction and HPLC with UV or fluorescence detectors, the latter used after a postcolumn reaction (115). Nine N-methylcarbamate and O-(methylcarbamoy1)oximepesticides and transformation products in groundwaters at 8 and 40 ppb were assayed using reversed-phase HPLC, postcolumn hydrolysis to yield CH3NH2, formation of an intense fluorophore with o-phthalaldehyde and mercaptoethanol, and fluorescence detection with 230 nm/418 nm excitation/emission wavelengths (175). Catalytic hydrolysis of N-methylcarbamates on an Aminex A-28 tetraalkylammonium anion exchanger was used to liberate methylamine prior to reaction with phthalaldehyde for HPLC fluorometric detection ( 3 4 4 ,while catalytic hydrolysis on a silica gel column was applied to the GC or HPLC determination of phenylurea herbicides and their aniline metabolites (125). Specific Procedures. Carbaryl was identified by chemical ionization MS with NH3 as the reagent as (75). Carbaryl was determined in polluted water by HPL8 with a postcolumn catalytic reactor and fluorogenic labeling (375). Carbaryl residues were determined in various samples as follows: in fruits or vegetables by extraction with CH2C12,cleanup on an alumina-AgNO column, and silica gel HPLC with dioxaneisooctane mobife phase (45); in wheat grain by methanol extraction and silica gel HPLC (86% recovery at 5 ppm) (16J); in pineapple using reversed-phase HPLC with fluorometric detection at 288 nm and by GC MS with NH3 chemical ionization and SIM (85); and wit 1-naphthol at 2 ppm in biological fluids using ethyl acetate extraction and reversed phase HPLC with fluorescence detection ( 1 0 4 . HPLC and GC/MS were compared for the determination of carbofuran and its metabolites in carrot (395). Carbofuran was determined in soil (0.4 ppm) with 90% recovery by methanol extraction, hexane-methanol-water (241) partition, and HPLC of the aqueous layer with UV detection at 280 nm (255). Gas chromatography with N-specific detection was applied to residue determinations of carbofuran and its carbamate metabolites in peppermint hay and oil at 0.05 and 0.1 ppm, respectively (205) and in rapeseed lants at 0.03-5 ppm (275). Carbofuran and carbosulfan resi&es in various crops, soil, and water were assayed by partition, column cleanup, and N-selective GC (295). Low recoveries from acidic crops were improved by replacing the water in the extraction solvent with a phosphate or borax buffer (285). Phenolic metabolites of carbofuran were determined in 12 crop matrices by acid hydrolysis, extraction, ethoxylation, partition into base, acidification, extraction, silica gel Sep-PAK cleanup, and GC/MS (335);in peppermint oil and hay by formation of heptyl ether derivatives and multiple ion detection MS (215);in hops by GC-GC after C18-HPLCcleanup and reaction with fluorodinitrobenzene (135); and by RP-HPLC as their 2,4-dinitrophenyl ether derivatives with UV detection at 280 or 300 nm (sensitivity limits 2-4 ng) (265). The followin analyses were devised for aldicarb and related compound resifues: aldicarb, thiofanox, and their metabolites in sugar beet leaves by GC with an N-P detector (55);aldicarb in tobacco by HPLC after oxidation to the sulfone (155); aldicarb, aldicarb sulfoxide,and aldicarb sulfone in strawberry fruits and plants, sugar beets, and soil by temperature gradient GC using an S-mode FPD detector (225); aldicarb, butocarboxim, and their metabolites by GC CI-MS (315);aldicarb and its sulfoxide, sulfone, oxime, an nitrile derivatives in groundwater by RP-HPLC with UV (200 nm) detection (30s); XAD-2 resin recovery of aldicarb and ita sulfoxide and sulfone from drinking water (1-10 ppb) prior to C18-HPLC with UV (254 nm) detection (325);a rapid two-step preconcentration procedure utilizing C 8-Sep-PAKsfor aldicarb determination HPLC with UV (254 nm) detection in water (5 ppb) by (385);aldicarb, aldicarg oxime, and aldicarb nitrile in water by GC/MS (415);aldicarb in water by HPLC using a nitrile-bonded column and CI-MS (425);and ppb levels of aldicarb and its sulfoxide and sulfone in water by capillary GC with an N-P detector (445). Bendiocarb insecticide was determined in soil by differential pulse polarography (185) and in soil and corn by GC with alkali flame ionization detection (405). LC/CI-MS (95) and LC MS using glass-lined stainless steel microbore columns (I were applied to the assay of ICP and CICP. Propoxur
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(Baygon) was determined in vegetables (0.5 ppm) by base hydrolysis, coupling with diazotized 4,4’-sulfonylbis(aniline), and solution colorimetry at 500 nm ( 3 4 , and in water by CIS-Sep-PAK extraction and HPLC-UV (272 nm) (245). Derivatives of phenmedipham and desmedipham with good GC properties were prepared by on-column degradation and methylation with N,N,N-trimethylaniliniumhydroxide (365). HERBICIDES AND PLANT GROWTH REGULATORS See also the previous section for some references on carbamate herbicides. General Procedures. Methabenzthiazuron and metribuzin were determined in soil, and these compounds plus dicamba and MCPA in water by HPLC (38K). Trifluralin, diallate, triallate, atrazine, barban, diclofop-methyl, and benzoylprop-ethylwere determined in sediment at ppb levels (47K) and in water at ppt levels (45K) by GC with EC or N-P detectors. Ten acidic herbicides were determined in sediment by GC of pentafluorobenzyl ester derivatives (46K). Nitrogen-containing pesticides were determined in biological material at 20-50 ppb levels by capillary GC/MS (32K). Nine dinitroaniline herbicides were separated by GC with an SE-32 capillary column and N-mode thermionic detector (22K). Fifteen phenylurea herbicides were determined in water and crop samples by adsorption HPLC and EC-GC after derivatization with heptafluorobutyric anhydride (15K). Urea and carbamate herbicides were chromatographed using an HPLC instrument with a wall jet electrode for electrochemical detection (5K). Solvent systems for the extraction of diclofop acid, picloram, simazine, and triallate from weathered field soils were compared (73K). Human lasma, urine, and gastric aspirate were analyzed for 2,5-D, MEPP, and chlorpyrifos by GC as part of a toxicological study in a case of fatal overdose (56K). Sixteen nitrophenols were determined in water (0.1-1 ppb) and sediment (10-50 ppm) by paired-ion HPLC (80K). Chlorophenoxy herbicides were extracted from soil using Amberlite XAD-4 resin (9OK) aad separated by HPLC using C18 and amino bonded columns (35K). Nitrophenols and phenoxycarboxylicacids were separated by HPLC as ion pairs (64K). The following methods of determination of phenoxycarboxylic acids were compared: GC after pentafluorobenzylation, HPLC of underivatized compounds in the ionsuppression and ion-pair modes, and HPLC of naphthacyl and methylmethoxycoumarin esters (65K). Chlorophenoxy herbicides were determined in wastewater and sludges by packed and capillary column GC with EC and MS detection (33K); in soil at 5-25 ppb by EC-GC of methyl esters (30K);and in wheat flour by EC-GC after derivatization with a-bromo2,3,4,5,6-pentafluorotoluene(28K). Multicolumn HPLC was applied to the trace analysis of 2,4,5-TP and 11other acidic herbicides in wheat at low ppb levels (66K). Chlorinated phenols were determined in herbicidal acids using on-line capillary GC/FTIR spectrometry (50K). Triazine herbicides were determined in water by GC with an N-P detector and by HPLC with a UV detector after solid phase extraction (61K, 76K). 1,3,5-Triazines in wastewater from the manufacture of ametryne were analyzed using HPLC with Cls- and NH2-bonded columns (21K). Plant hormones of the indole type were separated by C18-HPLC,detected by UV and fluorescence detectors, and identified by MS (87K). Proton NMR, IR, and mass spectra of indol-l-yl-, indol-2-yl-, and indol-3-ylaceticacids and their methyl esters were recorded and compared (79K). Indol-3ylacetic acid and seven related acids were reacted with phthalaldehyde and determined by spectrofluorometry (59113. Plant hormones were separated by countercurrent chromatography using a toroidal-coil planet cetrifuge (52K). HPLC was used for the simultaneous analysis of plant tissues for indol-3-ylacetic acid, 4-chloroindol-3-ylacetic acid, and 5hydroxyindol-3-ylaceticacid as their 2-methylindolo-a-pyrone derivaties (13K). Specific Procedures. GC analysis was used to measure 2,4-D in human blood, urine, hand rinses, and perspiration after occupational exposure (69K, 77K). An EC-GC method for 2,4-D in wheat was subjected to an interlaboratory study (72K). 2,4-D was determined in soil by capillary GC with ion-mobility detection (9K). MCPA and its two phenol metabolites were analyzed a t ppb levels in the environment nearby a bush killing treatment zone by EC-GC/MS using
PESTICIDES
pentafluorobenzyl derivatization (57K). Ametryn and three methylthioaminotriazine derivatives were determined in tropical root crops by GC with N-P or FPD detection (11K). GC and MS properties of ametryn and its N-dealkylated products were studied (12K). Sencor (metribuzin)was determined in plant material, soil, and water by GC with an N-specific alkali flame detector (36K) and in plant material by CIS-HPLC with UV (254 nm) detection (58K). Potatoes treated with chlorbromuron and dinoseb were analyzed by extraction, column cleanup, and EC-GC (62K). The Bleidner extraction method was modified to improve recovery of diuron residues from plants and soil (34K). Fluometuron was determined in soil a t 0.1-1 ppm using Ce-HPLC with UV (254 nm) detection (53K). Heptafluorobutyrylation of linuron and its metabolite 3,4-dichloroaniline was simplified for their EC-GC determination in carrot (85K). Tebuthiuron was determined in soil by HPLC using monuron as an internal standard for the extraction step (75K). Methoxuron and its breakdown product 3-chloro-4-methoxyaniline were determined by TLC and HPLC with fluorescence detection of dansyl derivatives (44K). Paraquat was determined in water (0.05 ppm) by CISSep-PAK extraction followed by RP-HPLC with W detection a t 257 nm (2K) and in blood or tissue by dialysis, addition of Na2S204,and spectrometry at 600 nm (71K). Differential pulse polarography determined diquat dibromide in wheat kernels at a sensitivity of 20 ppb (55K). Paraquat and diquat in urine were determined by HPLC-UV (290 nm) with rapid sample preparation involving ion-pair extraction on CISSep-PAKs (27K). Blood and urine containing paraquat and diquat at 1-70 ppm were analyzed by treatment with Reinecke salt, reduction of the derivatives with NiClz + NaBH4, and GC-FID of the perhydrogenated products (37K). Homogenized potato containing 0.05-5 ppm of paraquat or diquat was treated with NaBH4-ethanol, and the diene reduction products were extraded into hexane and analyzed by GC with N-P thermionic detection (86K). Difenzoquat in water (0.25-20 ppb) was trapped by an on-line enrichment column, desorbed, and analyzed by HPLC-UV (255 nm) (3K). Chlorsulphuron residues were determined in grain, straw, and een plants of cereals ( 7 0 and in soil (91K) by silica gel &LC with a photoconductivity detector. The preparation of soil samples without contamination was described (92K). Asulam, sulfanilamide, and sulfanilic acid were extracted from soil (0.2 pm) with methanol, separated by silica gel TLC, and detectefat a sensitivity of 10 n with fluorescamine (74K). A C18-HPLCmethod determine8 asulam, acetylasulam, and sulfanilamide in peaches at 0.1 ppm (40K). Pyridate was determined in cereals by HPLC-UV (48K). The main metabolite of pyridate, 3-phenyl-4-hydroxy-6chloropyridazine, was determined in maize leaf or stem by extraction, TLC, formation of the pentachlorobenzoylderivative, and EC-GC (43K), and in cereals by extraction, a three-step clean-up process, derivatization into 3-phenyl4,6-dichloropyridazine,and capillary GC-EC (49K). ClgHPLC was used to determine gibberellins in seeds (88K) and for analysis of acidic and conjugated gibberellins (41K). Highperformance TLC with densitometry was used to quantify gibberellin A3 and A4 + A, in fermentation broths (67K). Picloram residues in soil and water (2 ppb) were cleaned up by trapping on a C18-Sep-PAK and determined in underivatized form by cle-HPLC with UV (254 nm) detection (83K). Recoveries of picloram, its methyl ester, and hexazinone from C18-Sep-PAKswere increased when 5 mM tetrabutylammonium hydrogen sulfate was added to their solution in aqueous 4% acetic acid (82K). Hexazinone metabolites from rat-liver microsomes, peanut seedlings, and sugar cane have been identified by direct- robe MS of fractions separated by TLC or by GC/MS ( 6 3 2 Hexazinone residues from soil and water were separated on a C8-HPLC column, detected at 254 nm, and confirmed by GC/MS (14K). Ioxynil and bromoxynil residues were determined in barley at 50 ppb by acetone extraction; cleanup by solvent partition, GPC, and nitrile-bonded column LC; and reversed phase HPLC with UV and electrochemicaldetection (17K). Bromoxynil octanoate and metribuzin and their metabolite DADK in runoff water from wheat fields (20-200 ppb) were determined by CIS-HPLC-UV (16K). Field desorption MS and TLC identified DNOC in urine (78K). Dinoseb and DNOC
in water were determined by TLC and differential pulse polarography (60K). Negative chemical ionization MS quantitatively measured ethalfluralin and trifluralin in soil extracts (54K). A previously published colorimetric method for 3-amino-1,2,4-triazole in grain or meal was simplified and modified to lower the limit of detection to 0.05 ppm (26K). Gas chromatography was applied to the following herbicide determinations: soil-bound 3,4-dichloroaniline (a herbicide biodegradation product) extracted by the Bleidner technique (8983;endothal in human liver tissue, blood, and stomach contents (7K);3,6-dichloropicolinic acid in sugar beets at 0.05-1 ppm (25K);allidochlor in leeks (19K); glyphosate and aminomethylphosphonicacid in blueberries (31K);oryzalin in potato, soil, and water as the derivative formed with dimethylsulfinylanion and methyl or ethyl iodide (IOK);and triallate in grain pellets (18K).The following herbicide assays based on HPLC were described: glyphosate in soil and water (amine column and fluorescence detection) (29K); bentazon in crops and soil (20 ppb) with ion-pair extraction cleanup (1K);propanil in rice, potato, and water (C18column, 246 nm UV detection) (4K);and 10 ppb of 2,6-dichlorobenzonitrileand 2,6-dichlorobenzamide in aqueous samples (CIScolumn, 205 nm UV detection) without preliminary extraction or concentration (20K). The plant growth regulator 4-chlorophenoxyaceticacid was determined in mung bean sprouts (50 ppb) by EC-GC after extraction, partition, derivatization, and silica gel column cleanup (84K). HPLC with fluorescence detection was used for the analysis of grapes for residues of 1-naphthyleneacetic acid and related compounds (8K).Maleic hydrazide was determined in potato tubers by EC-GC after oxidation to 3,6-pyridazinedione (39K). Abscisic acid was quantified in plant extracts by Cle-HPLC-UV(260 nm) (52K),and by GC after cleanup on a silica gel Sep-PAK or Cle preadsorbent TLC plate and methylation (23K). &-(+)-Abscisic acid was determined by enzyme immunoassay after extraction from plant cells, silica gel TLC cleanup, and esterification (81K). The following analyses for indol-3-ylacetic acid (IAA) were described: comparison of the 2-methylindolo-a-pyrone fluorescence assay with HPLC and fluorescence detection (68K); IAA and abscisic acid in chestnuts by column chromatography on Sephadex G-10 and C1 -HPLC-UV (254 nm) (42K);IAA in soils by ion-pair HPLC f124K);IAA in pea and maize seedlings by capillary GC/MS (6K).
FUNGICIDES General Procedures. Captan, folpet, and captafol were best separated on a GC column of SP-2401 (17L) and were determined in fruits and vegetables using the multiresidue methods of Mills and Luke (18L). Eleven 4-aminotriphenylmethane fungicides were separated by C18-HPLCand detected at 600 nm (115).Vinclozolin, iprodione, procymidone, dichlozolinate, and their degradation product 3,5-dichloroaniline were determined in white must and wine extracts by RP-HPLC-UV (210 nm) (14L). Fungicide and insecticide residues in various crops a t 10-50 ppb levels were analyzed by OV-1 capillary column EC-GC (2L). Fungicides and 2aminobenzimidazole in surface water were determined by RP-HPLC-UV (280 nm) (37L). Thiabendazole (TBZ), ethoxyquin, and maleic hydrazide were determined in wastewater by HPLC with direct aqueous injection and fluorescence and electrochemicaldetection (3415). TBZ, o-phenylphenol, and biphenyl residues in citrus fruits were determined simultaneously without prior cleanup by C8-HPLC with UV or fluorescence detection (22L). Analytical methods for dithiocarbamate fungicide residues were reported as follows: a standard method for tobacco involving decompoeition of pesticides by heating with HC1 and SnClz, distillation of the resulting CSz into methanolic KOH, determination in fruits and spectrometry at 302 nm (11L); headspace GC methods for and vegetables by HPLC (19L); foodstuff analysis (20L);separations by HPLC using a micellar analysis of soil, onion, and tomato juice mobile phase (21L); by cryogenic concentration and FPD-GC (27L);and dimethyl dithiocarbamate degradation products by Cle-HPLC (9L). Specific Procedures. Metalaxyl residues were determined in plant tissue (38L) and soil (5L) using bioassay; in tomato (50 ppb) by ethyl acetate extraction and GC with N-P thermionic detection (36L);and de adation products of metalaxyl in lettuce and sunflower by f C , IR, NMR, and mass specANALYTICAL CHEMISTRY, VOL. 57,
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trometry (13L). Phenylmercury compounds were determined in soil, dust, and food at ppb levels by GC of phenylmercury derivatives on a column saturated with HgC12 (23L). Phenylmercuric acetate in seeds and water was separated and detected in the field by enzyme-inhibition and paper chromatography procedures (16L). Ferbam and its three degradation products were separated and detected by HPLC at 5 ppb, which corresponds to the FA0 criterion for analysis of dithocarbamates in food (1OL). Zineb in foliage was determined by silica gel TLC separation, detection with DCQ reagent, elution of the spot, and measurement of absorbance at 500 nm (29L). ETU, a degradation product of ethylenebis(dithiocarbamates), was determined in gra es, wine, and wheat by capillary GC of S-butyl-, Sbenzyl-, anftrifluoroacetyl derivatives (28L),and in berries and cigarette smoke concentrate as a volatile N,N'-dimethyl derivative by GC/MS and GC with an N-P detector (4L). PCP in mushrooms was determined by steam distillation, extraction of the distillate with CH2Cl ,and HPLC with a C8 column and 220-nm detection or EC-&C after derivatization with acetic anhydride (32L). Thiabendazole was determined in marmalades by HPLC-UV (305 nm) (15L)and in fruit peel by TLC with fluorometric quantification (7L). Benomyl was converted to carbendazim and determined by RP-HPLC on surgical gauze patches (39L). The captan metabolite tetrahydrophthalimide was determined in urine (10 ppb) by CHCI, extraction, Florisil column cleanup, and GC with an N-P detector (31L). Apples were analyzed for dithianon residues (50 ppb) by extraction, cleanup on silica gel, and RP-HPLC with detection at 250 nm (6L).Dazomet residues in vegetable crops (5-10 ppb) were determined by CH2CI2extraction, Florisil column cleanup, and HPLC on a CN-bonded column with 285 nm detection (33L). Rubigan (phenarimol) was extracted from apples (0.1-1 ppm) with acetonitrile, partitioned into CHC13, cleaned up on a Florisil-charcoal column, and determined by EC-GC (30L). Residue analysis of cymoxanil in grapes was carried out by a multidimensional multicolumn HPLC method (26L). Santoquin and diphenylamine were determined in apples (50 ppb) by ethyl acetate extraction and temperature programmed FID-GC (35L). Propiconazole and etaconazole in plants, soil, and water were determined by N-selective GC after alumina and GPC column cleanup (12L). Prochloraz residues in citrus fruits were determined by HPLC (24L),and propylenethiourea (the main metabolite of propineb) in rat tissues and fluids (25L),vinclozolin in soil (8L),and mepronil in soil (3L) by GC. PYRETHROIDS Analytical methods for pyrethroid insecticides were reviewed (13M). Halogenated synthetic pyrethroids were separated by TLC on A NO3-impregnated alumina plates developed with hexane-%enzene (45:55) and hexane-chloroform (6040); 0.1 ppm was the minimum detectable level in cleaned up extracts of tomato, fruit, and soil samples (22M). Pyrethroids were determined in crops, water, and soil (19M)and screened in fruits, vegetables, paprika, sugar beet root, and leaves (2M) by extraction, partition and column adsorption cleanup, and EC-GC. Pyrethrum extracts were analyzed on capillary columns with 0.1 Fm film thickness (18M). Natural and synthetic pyrethrins were characterized by EI, CI, and FI/FD mass spectra and computer averaged integrated FD mass spectrometry (9M). The HPLC of a series of pyrethroid insecticides and associated carbonyls was studied using a system equipped with an IR detector and 5 pm silica gel column eluted with acetonitrile-methylene chloride-heptane or 1-tetradecane-methylene chloride; log k' was linearly correlated with the log of the mole fraction of acetonitrile or tetradecane in the mobile phase (14M). HPLC was used for pyrethroid separations as follows: six pyrethrin esters found in extracts of pyrethrum flowers on double silica gel columns ( I I M ) ; cis and trans isomers of synthetic pyrethroids on reversed phase columns (8M); and enantiomers of pyrethroids on chiral ptationary phases (3M, 1OM) and as their (-)-1-(1-pheny1)ethylamide derivatives on silica gel columns (7M). Insect-proofing pyrethroids were determined on wool by extraction and HPLC with a CNbonded column (12M). Stability of natural pyrethrins separated by preparative HPLC was evaluated by GC and NMR spectrometry (5M). 8R
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Permethrin residues were determined on tomatoes and cucumbers by EC-GC (6M), on lettuce by HPLC with an on-line IR detector (15M),and in soil and water together with diflubenzuron by EC-GC ( 2 0 . Fenvalerate residues were determined in flowing seawater by GC with EC and N-P thermionic detectors (17M), and the GC determination of fenvalerate in processed tomato products was subjected to a five-laboratory collaborative study (21M). Decamethrin (delmethrin) was determined in chicks, adult quails, and eggs (4M) and in biological samples (lM) by EC-GC. Neopynamin (tetramethrin) and piperonyl butoxide were determined in shampoos and lotions by capillary column GC (16M). FUMIGANTS An air monitoring method involving sampling on Tenax-GC tubes, solvent desorption, and sample analysis by EC-GC was developed and validated for 1,3-dichloropropene, cis- and trans-1,2,3-trichloropropene,1,1,2,3-tetrachloropropene, 2,3,3-trichloro-2-propen-l-ol, and 1,1,2,2,3-pentachloropropane (7N). Seven fumigants were determined in stored grains by leaching with acetone-water (5:1), partitioning with isooctane, and GC analysis with 20% OV-101 and 20% OV-225-20% OV-17 (2:l) columns (3N). Ethylene dibromide was determined in citrus fruit (1-10 ppm) by homogenation with acetonitrile, extraction with hexane, and EC-GC; analysis of gas-phase samples from fumigation chambers was also reported (8N). Another GC method for ethylene dibromide in citrus fruits (5 ppb) involved steam distillation from benzene-water (15) and cleanup of the dried benzene distillate by addition of silica gel impregnated with fuming H2S04( 5 N . A portable gas chromatograph operated a t ambient temperature and fitted with a photoionization detector was used to determine amounts of ethylenee dibromide above 19 ppb in air (4N). A method was developed for determination of phosphine residues in wheat based on reaction of PH3 with AgNO, in aqueous solution to form a yellow chromophore that was measured by spectrometry at 400 nm ( I O N ) . Blood and tissues from a person who had ingested aluminum phosphide was analyzed for phosphine by headspace GC on a column of Porapak Q with N-P detection (2N). A portable gas chromatograph was used for direct monitoring of ambient air for ethylene oxide and ethylene dibromide ( I N ) . cis- and trans-1,3-Dichloropropenein whole rat blood was determined by GC and GC/CI-MS with selected ion monitoring (6N). Bromine residues in the soil and vegetable crops after soil fumigation with methyl bromide were determined by radioisotope-excited X-ray fluorescence spectrometry (9N). MISCELLANEOUS PESTICIDES Analytical methods for pesticides that were not easily classified in, or were omitted from, the sections above are reviewed in this part. The following analyses were reported: the acaricide benzomate in orange and apple at 1-2.5 ppm by C18-HPLC-UV (235 nm) (23P);imidazolidine-2-thione in vegetables by NH2-HPLC-UV (240 nm) after Sephadex LH-20 column cleanup (22P);inorganic As and methylarsenic compounds in water, urine, soil, and plants by GC and multiple ion detection MS after a hydride generation-heptane cold trap technique (21P);the insecticide rotenone and its degradation product rotenonone by RP-HPLC-UV (229 nm) with a limit of detection of 50 pg (19P);rotenone in water at 5 pg/L by RP-HPLC-UV (295 nm) after C18-Sep-PAKcleanup (5P); insect synergists in ambient air by RP-HPLC without interference from insecticides (1"); the insecticide butocarboxim and its sulfoxide and sulfone metabolites in vegetables, fruits, and soil (0.5 ppm) by C18-HPLC-UV (222 nm) after methanol extraction, silica gel column cleanup, NaOH hydrolysis, and derivatization of the resulting methylamine mildiomycin in plants with l-fluoro-2,4-dinitrobenzene(17P); and soil at 60-700 ppb by ion-pair RP-HPLC after extraction, cleanup, and reaction with fluorescamine (14P); the total analysis of amitraz insecticide and its metabolites in fruit and soil (0.05-1 ppm) by base hydrolysis t o 2,4-dimethylaniline, steam distillation/continuous extraction, acid/base partition cleanup, derivatization to the heptafluorobutyranilide, and EC-GC (11P);decoquinate in poultry feed (! ppm) by gradient elution HPLC with fluorescence detection (9P);atrazine metabolites from soil by HPLC, HPTLC, and GC/MS (7P);
PESTICIDES
8“‘“
eight insect growth re tors by HPLC (6P);the lampricides sodium I-nitro-&(tri uoromethy1)phenoxide (TMF) and niclosamide ethanolamine (Bayer 73) in water simultaneously by collection on a C 8-Sep-PAK,elution, and RP-HPLC-UV (330 or 254 nm) ( 4 4 ;and the hybridizing agent fenridazonpotassium (0.05-0.1 ppm) in wheat grain and straw by mild alkaline extraction, Cu-activated Chelex 100 column chromatography, liquid-liquid partition, and ion-pair RPHPLC-UV (285 nm) (2P). Residues of the coumarin anticoagulant rodenticides warfarin, coumatatralyl, bromadiolone, difenacoum, and brodifacoum were determined simultaneously in tissues by HPLC with fluorescence detection employing either postcolumn reaction with s-butylamine (12P) or an ion-pairing mobile phase (13P). A fluorometric CB-HPLC method for determination of brodifacoum in animal tissues was modified for analysis of fat and muscle (IOP).Racumin rodenticide was determined in soil and water (10-100 ppb) by RP-HPLC-UV (320 nm) after extraction with acetone, water, and HCl and cleanup by solvent partitioning and use of silica gel Sep-PAKs (20P). Chlorophacinone was determined in mouse tissue by HPLC on an “,-bonded column after acetonitrile extraction and Florisil column cleanup (1P). An EC-GP procedure was described for identification of 32 substituted phenols, including all 19 chlorophenols and the 11EPA consent decree phenols, based on formation of pentafluorobenzyl ethers (15P).Fifteen chlorophenols were analyzed in natural waters by in situ acetylation and EC-GC (16P). Phenol residues in lettuce, carrot, and apple were determined, after extraction and cleanup, by capillary GC-EC (BP). RP-HPLC, fluorometric, and colorimetric methods were evaluated for determination of residues of the bee repellent phenol in honey and beeswax after an initial steam distillation (3P).
INDUSTRIAL CHEMICALS RELATED TO PESTICIDES A large number of papers were published on the analysis of various samples for polychlorinated biphenyls (PCBs), usually in the presence of organochlorine (OC) pesticides. Recent advances in analyses of PCBs in environmental and biological media (31Q) and PCB structure-activity relationships (37Q) were reviewed. All 209 mono-, di-, tri-, tetra-, penta-, hexa-, and heptachlorobiphenylswere synthesized and their spectrometric and chromatographic properties reported (23Q). A BASIC computer routine was presented for calculation of PCB concentrations using the individual peak-weight percent method and GC on a 5% OV-101 column (246). A laboratory data base for computer-assisted isomer-specific determinations of PCBs used a retention index system with n-alkyl trichloroacetates as marker compounds (39Q). Six technical Aroclors were separated into individual chlorobiphenyls that were identified by fused silica gel capillary column GC/MS (47Q). GC/high-resolution MS and MS/MS were compared for detection of PCBs and tetrachlorodibenzofuran (48Q). Time-pro rammed limited mass scan GC/MS for PCB analysis invofved selection of discrete portions of the mass range, adjusted automatically during chromatography to match elution times, to monitor the presence of characteristic groups of ions (509). Cyclodiene insecticides were determined in the presence of PCBs by photoisomerization reactions (28Q). Perchlorination to decachlorobiphenylwith SOzCl in the presence of AlCl allowed rapid determination of PeBs by EC-GC (46Q). bC pesticides and PCBs were cleaned up prior to GC analysis by gel permeation chromatography with the mobile phase methylene chloride-cyclohexane (43Q), by chromatography of fat samples on columns of silica gel (45Q),and on columns of silica gel containing 10% water (on-line method for extraction and isolation from meat and fish) (44Q). An analytical method for the determination of PCBs in motor and transformer oils, developed by the NBS in the certification of a standard reference material, involved preparative scale HPLC to remove interferences and high-resolution capillary GC on a nonpolar wall coated open tube with EC or Hall electrolytic conductivity detectors (29Q). The analysis of PCBs in oil was evaluated by an NBSIASTM round robin study involving 11oils and 19 laboratorles (3Q). Several GC methods for PCBs in oil were compared (14Q). Transformer oils were screened for PCBs by nondisperse
X-ray fluorescence spectrometric analysis of chlorine (17Q). Capillary EC-GC determined PCBs in electrical insulating liquids after dilution and Florisil column cleanup (40Q). The following additional determinations of PCBs, most by EC-GC after extraction and adsorption column cleanup, were described PCBs and DDE in human body fluids and infant formula (196);PCBs and OC pesticides in bovine serum (4Q) with an interlaboratory study (5Q);in sediment by pyrolysis GC(MS (20Q) and capillary column GC (276); in marine sediment by GC/negative CI-MS (15Q);field measurement of PCBs in soil and sediment using a portable gas chromatograph (42Q);isolation by steam distillation from fatty foods also containing OC pesticides (18Q);in herring meat and liver (1Q);in human milk and butter by capillary GC (38Q);in monkey milk and tissues (21Q);in industrial and municipal wastewaters also containing OC pesticides (22Q);in air samples with collection on polyurethane foam (25Q);in pigments (2Q); in biotic and abiotic marine compartments (9Q);in sewage sludges using packed and capillary column GC and MS (11Q); and in peregrine falcon eggs (30Q). Several agricultural chemicals were examined for contamination by polychlorinated dibenzo-p-dioxins (PCDDs) and related compounds by GC/MS (7Q). All possible PCDD isomers containing four or more C1 substituents were prepared by micropyrolysis of chlorophenates and their capillary GC/MS properties were studied (6Q). Concentration of solutions of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) by combined refluxing + nitrogen evaporation, vacuum evaporation, and nitrogen evaporation were compared; substantial losses were obtained only by evaporation to dryness under nitrogen (26Q). PCDD residues were determined in biological samples by C18-HPLC-UV(235 nm) using polycyclic aromatic hydrocarbons as calibration standards (36Q). Fish and deer samples were analyzed for TCDD by GC at low ppt levels (12Q). Soil and vapor samples were analyzed for TCDD by GC/MS (16Q). PCDDs and dibenzofurans were identified in human samples by capillary GC/MS (34Q). TCDD was determined at ppt levels in wastewater by extraction, cleanup on silica and alumina columns, and GC/MS (32Q, 51Q). 2,3,7,8-Tetrachlorodibenzo-p-dioxin and -tetrachlorodibenzofuran were determined in a soot sample from a transformer explosion by GC/MS after extraction and cleanup by carbon-celite, silica gel, and Zorbax ODS and SIL HPLC columns (41Q). TCDD in sugar (1ppt) was determined by GC high-resolution MS (49Q). dhthalate esters were separated from PCBs and OC pesticides on dual alumina and silica gel columns as part of an EC-GC analysis of environmental samples (35Q). Phthalate esters were determined in sediment at 1-5 ppb by GC/SIMMS (33Q). Polychlorinated naphthalenes (PCNs) in the presence of PCBs were determined in sediment by steam extraction to separate OC compounds from the matrix, hydrodechlorination of PCNs (but not PCBs) by in situ generation of “nickel boride” by treatment of NiCl, with NaBH4 in 2-propanol, and measurement of naphthalene content of the mixture on a capillary GC column (13Q). Polychlorinated terphenyls were analyzed in environmental samples by capillary GC/MS, silica gel HPLC-UV (207 nm), silica gel TLC, and perchlorination/GC (8Q). Polybrominated biphenyl residues were determined in animal tissue by GC after extraction with CHCl3-methanol(2:1) for liver and CH2C1, for adipose tissue (log). LITERATURE CITED 0ENERAL
(IA) Blalcher, G.; Pfannhauser, W.; Woidich, H. Recent Dev. Food Anal., PrOC. €or. Conf. Food Chem., lsf 1987 (Publ. 1982), 437-442. Chem. Absfr. 1983, 98, 15528a. (2A) Bluethgen, A,; Heeschen, W.; Nljhuls, H. I n ”Challenges to Contemporary Dairy Analytical Technlques”; Royal SOC.Chem.: London, 1984 pp 206-235. (3A) Bottomley, P. Anal. Proc. (London) 1983, 20, 401-404. Chem Absfr. 1983, 9 9 , 207941~. (4A) Cairns, T.; Siegmund E. G.; Jacobsen, R. A.; Barry T.; Petzinger, G.; Morris, W.; Helkes, D. Blamed. Mass Specfrom. 1983, 70,301-315. (5A) Carl, M. I n “Challenges to Contemporary Dairy Analytical Techniques”; Royal SOC.Chem.: London, 1984 p 316. (6A) Chau, A. S. Y.; Lee, H. B. I n “Anal. Pestlc. Water”; CRC: Boca Raton, FL, 1982; Vol. 1, pp 25-81. (7A) Conacher, H. B. S. I n “Chem. World Food Supplies, New Front. Chemrawn 2, Invited Pap. Int. Conf.”; Pergamon: Oxford, UK, 1982 (Publ. 1983); pp 505-514. ANALYTICAL CHEMISTRY, VOL. 57, NO. 5, APRIL 1985
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PESTICIDES (8A) Ebing, W. I n “Pestic. Chem. Hum. Welfare Envlron. Proc. Int. Congr. Pestic. Chem, 5th l982”, (Pub. 1983), Pergamon: Oxford, UK; Voi. 4, pp 55-60. (9A) Fishbein, L. I n “Environ. Specimen Banking Monk Reiat. Banking Proc. Int. Workshop 1982”, (Pub 1984), NiJhoff Hingham. MA; pp 287-303. (IOA) Games, D. E. Prog. Pestic. Blochem. Toxicoi. 1983, 3, 367-400. (1 I A ) Horwitz, W. I n “Challenges to Contemporary Dairy Analytical Techniques”; Roy. SOC.Chem.: London, 1984; pp 1-13. (12A) IUPAC Applied Chem. Div. (USA). Pure Appl. Chem. 1084, 56, 945-956. (13A) IUPAC Commission on Pesticide Chemistry. Pure Appl. Chem. 1084, 56, 1131-52. (14A) Lauren, D. R.; Holland, P. T. Chem. New. Zealand 1983, 4 7 , 81-83. (15A) Lee, H. 8.; Chau, A. S. Y. Kawahara, F. I n “Anal. Pestlc, Water”; CRC: Boca Raton, FL; Vol. 2, pp 1-60. (16A) McCown, S. M.; Manos, C. G.; Pltzer, D. R.; Earnest, C. M. Af78/ySf (London) 1982, 707. 1393-1406. (17A) Muecke, W. frog. fesfic. Blochem. Toxlcol. 1083, 3,279-368. (16A) Rappe, C. Environ. Scl Technol. 1084, 78, 78A-90A. (WA) Ripley, B.; Chau, A. S. Y. I n “Anal. Pestic. Water”; CRC: Boca Raton, FL, 1962; Vol. 3. pp 1-182. (20A) Roseboom, H. Food Scl. Technol. 1984, 7 7 , 489-532. (21A) Schwedt, G. Z . Lebensm.-Unfers. Forsch. 1084, 779, 183-189. (22A) Seiber, J. N. Baslc Life Scl. 1982, 2 7 , 219-234. (23A) Strachan, W. M. J.; Glooschenko, W. A.; Maguire, R. J., I n “Anal. Pestic. Water”; CRC: Boca Raton, FL, 1982; Vol. 1, pp 1-23. (24A) Thier, H P. I n ”Pestic. Chem.: Hum. Welfare Environ. Proc. Int. Congr. Pestic. Chem., 5th 1982”; Pergamon: Oxford, UK, 1963; Vol. 4, pp 89-94. (25A) Zweig, G. I n “Modern Methods of Food Analysis. IFT Basic Symp. Series, 1983”; Avi: Westport CT, 1984; Chapter 14, pp 339-368. BOOKS AND REVIEWS (le) Albaiges, J., Ed. “Analytical Techniques in Environmental Chemistry”; Pergamon Press: Oxford, UK, 1982 473 pp. (28) Amer. Assoc. Cereal Chem. 6th Ed. of Approved Methods”; Amer. Assoc. Cereal Chem.: St. Paul, MN, 1983; 1084 pp. (38) Chau, A. S. Y., Afghan, 8. K., Eds. ”Analysis of Pesticides in Water”; CRC Press: Boca Raton, FL, 1982 Voi. 1-3, 202 pp, 238 pp, 248 pp, (48) Eisenbrand, 0.ARC Scl. Publ. 1983, 45, 275-276. (5B) Fest C.; Schmidt, K. J. ”The Chemistry of Organophosphorus Pesticides”, 2nd ed.; Springer-Verlag: Berlin, 1982; 360 pp. (6B) Fischbein, L. J. Chromatogr. Llbr. 1983, 2 2 8 , 435-458. (78) Food and Drug Administration (U.S.). “Pesticide Analytical Manual”; FDA: Washington, DC, 1982; Voi. 2, 1643 pp. (8B) Hassall, K. A. “The Chemistry of Pesticides: Their Metabolism, Mode of Action and Uses In Crop Protection”; Verlag Chemie: Weinhelm, Fed. Rep. Ger., 1982; 372 pp. (9B) Henriet, J., Ed. “Pesticide-CIPAC Standardized Methods of Analysis and Proceedings Symposium Papers”; CIPAC Ltd.: Hertfordshlre, UK, 198 I; VOl. 3, 399 pp. (lOB) Kempter, G.; Jurnar, A. “Chemistry of Organic Plant Protective Agents and Pesticides” 2nd ed.; Dtsch. Verlag Wlss.: Berlin, Fed. Rep. Ger. 1983; 150 pp. ( I I B ) Khan, S. ResMue Rev. 1982, 84, 1-25. (128) MacDonald, D., Ed. “International Pesticide Directory 1983, 3rd Ed.”; MacDonakl Pubi.: Uxbridge, UK, 1983; 79 pp. (138) E. E. J., Ed. ”Pharmacological and Chemical Synonyms: A Collection of Names of Drugs, Pesticides and Other Compounds”, 7th ed.; Excerpta Medica: Amsterdam, Neth. 1983; 514 pp. (148) Marr, I.L.; Cresser, M. S. Environmental Chemical Analysis”; Malcolm S.: Blackie, Glasgow, 1982; 272 pp. (15B) Smith, A. E.; Grover, R. In “Anal. Pestic. Water ”; CRC Boca Raton FL, 1982; VOl. 3, pp 183-211. (I6B) Smith, A. E.; Muir, D. C. C.; Grover, R. I n ”Anal. Pestlc. Water”; CRC Boca Raton, FL, 1982; Voi.3, pp 213-239. (178) Soderlund, D. M.; Sanborn, J. R.; Lee, P. W. Prog. festic. Blochem. TOXlCOl. 1983, 3, 401-435. (18B) Tucker, R. E., Young, A. L., Gray, A. P., Eds. “Human and Environmental Risks of Chlorinated Dioxins and Related Compounds”; Plenum Press: New York, 1963; 833 pp. (l9B) Vonk, J. W. frog. festlc. Blochem. Toxlcoi. 1983, 3 , 111-162. (208) Weed Science Society of America “Herbicide Handbook”, 5th ed.; Weed Scl. Soc. Am.: Champaign, IL, 1983; 515 pp. (218) Young, R. W. Dev. FoodAnal. Tech. 1984, 3 , 145-174. (229) Zweig, G., Sherma, J., Eds. ”Pyrethroids and Other Pesticides”; Vol. 13, Analyticai Methods for Pesticides and Plant Growth Regulators; Academic Press: Orlando, FL, and San Dlego, CA, 1984; 312 pp.
SAMPLINQ AND CLEANUP (IC) Agostlano, A.; Caseiii, M.; Provenzano, M. R. Water, Alr, Soil foliut. 1983, 79, 309-320. (2C) Balischmitter, K. Pure Appl. Chem. 1083, 55, 1943-1956. (3C) Billings, W. N.; Bidleman, T. F. Atmos. Envlron. 1983, 17. 383-391. (4C) Bruner, F.; Crescentini, G.; Mangani. F. Petty, R. Anal. Chem. 1983, 55, 793-795. (5C) Chiavari, 0.; Pastoreill. L.; Vitaii, P. Fresenius’ 2.Anal. Chem. 1984, 377. 130-131. (6C) Dao, T. H.; Lavy, T. L.; Dragun, J. Residue Rev. 1983, 87, 91-104. (7C) DeRoos, F. L.; Wensky, A. K. EPA Report EPA-600/7-84-060 1984; available from NTIS. ORDER No. PB84-215482; 25 pp. (8C) . . Easter, E. P.; Leonas, K. K.; DeJonge, J. 0. Bull. Envlron. Contam. Toxlcol. i983, 37,736-44. (9C) Flguerola, F. E.; Shibamoto, T. Agrlc. Blol. Chem. 1983, 47, 2933-2934.
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(IOC) Friedman, L. C.; Fishman, M. J.; Boyie, D. K. J. Test. Eva/. 1084, 12, 114-1 18. ( l l c ) Fuchsbichier. G. Lsndwlftsch. Forsch. 1983, 36, 130-139. Chem. Absfr. 1084, 700, 119401e. (12C) Giliespie, A. M.; Walters, S. M. J. Assoc. Off. Anal. Chem. 1984, 67, 290-294. (13C) Gretch, F. M.; Rosen, J. D. J. Assoc. Off. Anal. Chem. 1984, 67, 108-1 11, (14C) Gretch, F. M.; Rosen, J. D. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 783-789. (15C) Hodgson, D. W.; Thompson, J. F.; Watts, R. R. J. Off. Anel. Chem. 1082. 65. 94-102. (16C) Holland, P. T.iMcGhie, T. K. J. Assoc. Off. Anal. Chem. 1983. 66, 1003-1008. (17C) Hopper, M. L. J. Agrlc. Food Chem. 1982, 30, 1038-1041. (18C) Hulpke, H. Fresenlus’ Z. Anal. Chem. 1983, 374, 745-750. (19C) Onishi, H. Bunsekl Kegaku 1083, 3 2 , E251-E258. Chem. Absb. 1983, 9 9 , 145790m. (20C) Krause, R. T.; August, E. M. J. Assoc. Off. Anal. Chem. 1083, 66, 1018-1022. (21C) Krzymien, M. E. Inf. J. fnvlron. Anal. Chem. 1082, 73,69-84. (22C) Leesch, J. G. J. €con. fntomol. 1982, 75, 899-905. (23C) Levesque, D.; Mallet, V. N. Int. J. Envlron. Anal. Chem. 1083, 76, 139-147. (24C) Lewis, R. W.; Visscher, S. N. flenf Growth Regui. 1082, 7 , 25-30. (25C) Liu, S.; Tiliberg, E. fhysloi. flenf. 1983. 5 7 , 441-447. (26C) Luke, 9. 0.; Richards, J. C.; Dawes, E. F. J. Assoc. Off. Anal. Chem. 1084, 6 7 , 295-298. (27C) Luke, M. A.; Doose, G. M. Bull. Environ. Contam. Toxlcol. 1984, 3 2 , 651-656. (28‘2) Luke, M. A.; Doose, G. M. M i . Environ. Confam. Toxlcol. 1983, 30, 110-1 16. (29C) Mac Leod, K. E.; Hanisch, R. C.; Lewis, R. G. J. Anal. Toxlcol. 1982, 6, 38-40. (30C) McKone, H. T.; Daub, A. Anal. Chem. Symp. Ser. 1983, No. 74, 497-503. (31C) Narang, A. S.; Vernoy, C. A.; Eadon. G. A. J . Assoc. Off. Anal. Chem. 1983, 66, 1330-1334. (32C) Nash, R. 0. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 199-203. (33C) Neldert, E.; Saschenbrecker, P. J . Assoc. Off. Anal. Chem. 1084, 67, 773-775. (34C) Nieisen, P. 0. Chromatographla 1984, 18, 323-325. (35C) Papadopouiou-MourkMou, E.; Iwata, Y. Chromafogrephla 1983, 77, 695-700. (36C) Popl, M.; Tatar, V.; Voznakova, 2. Fresenlus’ 2.Anal. Chem. 1982, 313, 137-140. (37C) Pyysalo, H. fesffc Chem .: Hum. Wdfare Environ Roc. Inf Congr Pesflc. Chem. 5th 7962 1983, 4, 123-128. (38C) Radian Corp. Report 1984 EPA-600/4-84-053; NTIS Order # PB84206572; 474 pp. (39C) Rohleder, H.; Gorbach, S. fesfic. Chem.: Hum. Welfare fnviron. R o c . Inf. Congr. festlc. Chem., 5fh 7982 1983, 4 , 43-48. (40C) Smart, N. A. Ana/ysf (London) 1984, 109, 761-766. (41C) Sneison, J. T. festlc. Chem.: Hum. Welfare Envkon. froc. Inf. Congr. fesfic. Chem., 5th 7982 1983, 4 , 13-22. (42C) Solomon, J. CA 1,155,317, 18 Oct. 1983; 23 pp. Chem. Absfr. 1984, 700. 48077r. (43C) Sonchik, S.; Madeleine, D.; Macek, P.; Longbottom, J. J. Chromatogr. SCi. 1984. 22. 265-271. (44c) sonoboe, H.; Sakuma, S.; Yamada, K.; Kawasaki, M.; Katayama, H.; Kuroiwa, Y. foc. Conv. Insf. Brew. (New Zealand Secflon) 1982, 77fh, 56-69. Chem. Absfr. 1083, 98, 105650~. (45C) Suprynowlcz, 2.; Buszewskl, 8.; Pomorska. K. Poi. J. Chem. 1981, 5 5 , 2123-2127. Chem. Absh. 1983, 9 9 , 34403t. (46C) Thier, H.-P. Lebensmiftelchem. Qerlchtl. Chem. 1983, 37, 114-1 16. (47C) Van Dyk, L. P.; Lotter, L.; De Beer, P. R.; De Kierk, A.; VilJoen. A. J. Prinsioo, S. M. Analyst (London) 1983, 708, 748-753. (48C) Ware, G. W.; Estesen, B. J.; Buck, N. A. Bull. Envlron. Contem. Toxi d . 1082, 2 8 , 748-751. (49C) Wheeler, W. B.; Edeistein, R. L.; Thompson, N. P. festlc. Chem.: Hum. Welfare Envlron Roc. Inf Contgr. Pesflc Chem 5th 7982 1983, 4.49-54. (50C) Yeboah, P. 0.; Kiigore, W. W. Bull. Envlron. Contam. Toxicol. 1984, 33, 13-19. (51C) Yeboah, P. 0.; Kiigore, W. W. Bull. Environ. Confam. Toxicol. 1984. 3 2 , 629-634. (52C) Yurawecz, M. P.; Puma, 9. J. J. Assoc. Off. Anal. Chem. 1983, 66, 241-247.
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QAS CHROMATOQRAPHY (QC)
(ID) Attygale, A. B.; Morgan, E. D. Anel. Chem. 1083, 55, 1379-1384. (2D) Auk, J. A.; Spurgeon. T. E. J. ASJOG.Off. Anel. Chem. 1084, 6 7 , 264-269. (3D) Balm, M. A.; Hili, H. H. W C CC, J. Hlgh Resoluf. Chromafogr. Chro. k f o g r . Commun. 1083, 6 , 4-10. (40) Barry, T. L.; Petzlnger, G.; Geltrnan, J. Bull. Environ. Contam. Toxlcol. 1982, 2 9 , 611-614. f5D) Betowski. L. D.: Webb, H. M.: Sauter. A. D. Biomed. Mass. SReCtfOm. ’ 1983, i o , 389-3%. (6D) Burchili. P.; Herod, A. A.; Marsh, K. M. Prltchard, E. Weter Res. 1083,
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(7D) Cairns, T.; Siegmund, E. G.; Froberg, J. E. Bull. Environ. Contam. Toxlcol. 1084, 32,187-194. (8D) Cammann. K.: Lendero, L.: Feuerbacher, H.; Baiischmlter, K. Fresenlus ’ ‘ 2.Anal. C k m : 1983, 316, 194-200. (9D) Carson, L. J. J. Assoc. Off. Anal. Chem. 1083. 66. 1335-1344.
PESTICIDES (10D) Dan, J. L. Anal. Chem. 1984, 56, 2687-2692. (11D) Dan, J. L. Bull. Envlron. Contam. Toxlcol. 1983, 3 0 , 492-496, (12D) Dan, J. L. HRC CC, J. H@hResolut. ChfOmatOgr. ChrOmatOgr. Commun. 1983, 6, 480-487. (13D) Deleu. R.; Copin, A. HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun. 1984, 7 , 338-339. (14D) Erickson, D. H. Chem. Biomed. Environ. Instrum. 1983, 72, 397-408. (15D) Fehrlnger, N. V.; Waiters, S. M. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 91-95. (16D) Goebel, H.; Stan, H. J. J. Chromatogr. 1983, 279, 523-532. (17D) Hoggei L. R.; Olson, D. J. H. Ind. Res. Dev. 1982, 2 4 , 144-149. (18D) Holland, P. T.; McGhle, T. K.; McGaveston, D. A. ”Pestlc. Chem.: Hum. Welfare Environ R o c . Int , Congr festlc Chem ., 5th 7982 1983, 4 , 73-78. (19D) Hopper, M. L. J. Chromatogr. 1984, 302, 205-219. (20D) Hunt, 0. T.; Hoyt, M. P. HRC CC J. Hlgh Resolut. Chromatogr. Chromatogr. Commun. 1982, 5 , 291-298. (21D) Kafadar, K.; Eberhardt, K. R. J. Res. Natl. Bur. Stand. 1983, 8 8 , 37-46. (22D) Kalaslnsky, K. S. J. Chromatogr. Scl. 1983, 2 1 , 246-253. (230) Kapila, S.; Bornhop, D. J.; Manahan, S. E.; Nlckell, G. L. J . ChromatOgr. 1983, 259, 205-210. (240) Macholz, R.; Knoll, R.; Kujawa, M. Lange, R. 2. Gesamte Hyg. Ihre Grenzgeb. 1983, 2 9 , 336-339. Chem. Abstr 1983, 9 9 , 189058h. (25D) Macholz, R.; Knoll, R.; Kujawa, M.; Nickel, B. Z.Gesamte Hyg. Ihre Qrenzgeb. 1983, 2 9 , 340-343. Chem. Abstr. 1983, 9 9 , 189059). (26D) Mangani, F.; Bruner, F. Chromatographla 1983, 17, 377-380. (27D) Mangani, F.; Mastrogiacomo, A. R.; Marras, 0. Chromatographla 1982, 75; 712-716. (260) Moler, G. F.; Delongchamp. R. R.; Mitchum, R. K. Korfmacher, W. A,; Pearce, 8. A. Chlorlnated Dloxlns Dlbenzfurans Total Environ., (froc. Symp .) 7982 1983, 287-320. (29D) Moseley, M. A.; Pelllzzarl, E. D. HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun. 1982, 5 , 404-412. (30D) Moye, H. A.; Dyrup, C. L. J. Agrlc. FoodChem. 1984, 3 2 , 192-195. (31D) Nakamura, A.; Tanaka, R.; Kashlmoto, T. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 129-132. (32D) Nitz, S.; Moza, P.; Korte, F. J. Agrlc. Food Chem. 1982, 3 0 , 593-596. (33D) Poole, C. F.; Schuette, S. A. HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun 1983, 6 , 528-549. (34D) Rinderknecht, F.; Wenger, B. HRC CC, J. High Resolut. Chromatogr. Chmmatogr. Commun. 1983, 6, 422-428. (35D) Rlpley, B. D.; Braun, H. E. J. Assoc. Off. Anal. Chem. 1983, 66, 1084- 1095. (36D) Ryarl, P. A.; Denne, D. R.; Wakefield, K. C. J.; Warburton, G. A.: Hazelby, D. Int. J. Mass Spectrom. Ion fhys. 1983, 48, 283-266. (37D) Saleh, M. A. J. Agric. FoodChem. 1983, 3 1 , 748-751. (380) Schneider, J. F.; Bourne, S.; Boparal. A. S. J. Chromafogr. Scl. lg84, 22. 203-206. (390) Schutjes, C. P. M.; Vermeer, E. A.: Scherpenzeel, G. J.; Baliy, R. W.; Cramers, C. A. J. Chromatogr. 1984, 289, 157-162. (40D) Slu, K. W. Michael; Aue, W. A. Mlkrochim. Acta 1983, 1 , 419-430. (41D) Stan, H.J.; Goebel, H. J. Aufom. Chem. 1984, 6, 14-20. (42D) Stan, H.J.; Steinbach, e. J. Chromatogr. 1984, 290, 311-319. (43D) Stan, H.J.; Goebel, H. J. Chromatogr. 1983, 268, 55-69, (44D) Stan, H.J.; Mrowitz, D. J. Chromatogr. 1983, 279, 173-167. (45D) Stout, S. J.; Steller, W. A. Horned. Mass Spectrom. 1984, 7 7 , 207-210. (46D) Verga, G. R. J. Chromatogr. 1983, 279, 657-665. (47D) Wells, D. E.; Cowan, A. A. J. Chromatogr. 1983, 279, 209-216. (48D) Wells G. Anal. Chem. 1983, 5 5 , 2112-2115. (490) Wells, G. HRC CC , J. High Resolut Chromatogr Chromatogr Commun. 1983. 6, 651-654. (5013) Zenon-Roland, L.; Agneessens, R.; Nangniot, P.; Jacobs, H. HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun. 1984, 7 , 480-484. (51D) Zerezghi, M.; Mulligan, K. J.; Caruso, J. A. J. Chromatogr. Scl. 1984, 2 2 , 348-352.
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HIQH-PERFORMANCE LIOUID CHROMATOQRAPHY(HPLC) ( E ) Apffel, J. A.; Brinkman, U. A. T.; Frel, R. W.; Evers, E. A. I. M. Anal. Chem. 1983, 5 5 , 2280-2284. (2E) Bagon, D. A.; Warwlck, C. J. Chromatographla 1982, 76, 290-293. (3E) Braumann, T.; Weber, G.; Grlmrne, L. H. J. Chromatogr. 1983, 261, 329-343. (4E) Conerill, E. 0.; Byast, T. H. “Liquid Chromatography Environmental Analysis”; Lawrence, J. F., Ed.; Hutnana: Clifton, NJ, 1984, pp 77-114. (5E) Daldrup, T.; Mlchalke, P.; Boehme, W. Chromatogr. News/. 1982, 10 (l), 1-7. (6E) De Kok, A.; Geerdlnk. R. B.; Brlnkrnan, U. A. T. Chromatographla 1982, 16, 237-241. (7E) Dlmson, P. Llq. Chromatogr. H f L c Mag. 1983, 7, 236-237. (8E) Ding, X. D.; Krull, I . S. J. Agrlc. Food Chem, 1984, 3 2 , 662-628. (9E) Dong, M. W.; DlCesare, J. L. J. Chromatogr. Scl. 1882, 2 0 , 517-522. (10E) Donkerbroek, J. J.; Gooijer, C.; Velthorst. N. H.; Frel. R. W. Int. J. Envlron. Anal. Chem. 1983, 75, 261-301. (1 1E) Goewl, C. E.; Kwakman, P.; Frel, R. W.; Brlnkman, U. A. T.; Maasfeld, W.; Seshadrl, T.; Kenrup, A. J. Chromatogr. 1984, 284, 73-86. (12E) Kirkbrlght, G. F.; Mulllns. F. 0. P. Anal. Chlm. Acta 1984, 756, 279-282. (13E) Krause, R. T. J. Chromagotr. 1983, 255, 497-510. (14E) Levsen, K.; Schaefer, K. H.; Freudenthal, J. Chromatogr. Rev. 1983. 27, 51-60. (15E) Maye, H. A.; Mlles, C. J.; Scherer, S. J. Agfic. FoodChem. 1989, 31, 69-72.
(16E) Podowski, A. A.; Feroz, M.; Mertens, P.; Khan, M. A. Q. Bull. Envlron. Contam. Toxlcol. 1984, 3 2 , 301-309. (17E) Prince, J. L. J. Agric. FoodChem. 1984, 3 2 , 1184-1186. (18E) Slut, V.; Palmer, M. V. J. Chromatogr. 1983, 270, 309-312. (19E) Voyksner, R. D.; Bursey, J. T. Anal. Chem. 1984, 56, 1582-1567. (20E) Voyksner, R. D. Bursey, J. T.; Peliizzari, E. D. Anal. Chem. 1984, 5 6 , 1507-1514. (21E) Waiters, S. M. J. Chromatogr. 1983, 259, 227-242. (22E) Walters, S. M.; Gllvydis, D. M. Llq. Chromatogr. HPLC Mag. 1983, 1 , 302-304. (23E) West, S. D.; Dorulla, 0. K.; Poole, 0. M. J. Assoc. Off. Anal. Chem. 1983, 66, 111-114. (24E) Wollmann, H.; Bauer, H.; Voelter, W. Mikrochlm. Acta 1982, II, 89-94.
THIN-LAYER CHROMATOQRAPHY (TLC) (1F) Cserhati, T.; Orsl, F. PeriodPolytechn. Chem. Eng. 1982, 26. 111-119. Chem. Abstr. 1983, 98, 84774q. (2F) Fogy, I.; Allmaler, G. M.; Schmid, E. R. Int. J. Mass Spectrom. Ion fhys. 1983, 48, 319-322. (3F) Gupta, S.; Rathore, H. S.; Ali, I.; Ahmed, S. R. J. Llq. Chromatogr. 1984, 7 , 1321-1340. (4F) Hltos, P. festlc .-CIfAC Methods R o c . Ser . 1981, 3 , 32-50. (5F) Jackson, D. L.; McWha, J. A. J. Chromatogr. 1983, 267, 242-245. (8F) Janos, E.; Cserhatl, T. Acta fhflopath. Acad. Scl. Hung. 1982, 77, 343-346. Chem. Abstr. 1983, 99, 153743~. (7F) Kovac. J.; Kurucova, M.; Batora, V; Tekel, J.; Strniskova, V. J . Chromatogr. 1983, 280, 176-180. (8F) Makhubalo. J.; Malnga, A.; Phlri, A. J. Chromatogr. 1984, 284, 518-522. (9F) Ohlsson, S. V.; Hintze, W. W. HRC CC, J. High Resolut. Chromatogr. Chromatogr. Commun. 1983, 6, 89-94. (1OF) Pfelffer, R.; Stahr, H. M. Adv. Thln Layer Chromatography (froc. Slenn. Symp .), 2nd 1980 1982, 541-556. (11F) Renvall, S.; Akerblom, M. Var Foeda , 1982, 34 (Suppl. 3), 240-247. Anal. Abstr. 1983, 45, 1G33. (12F) Sherma, J.; Boymel, J. L. J. Liq. Chromatogr. 1983, 6 . 1183-1192. (13F) Sherma, J.; Getz, M. E. Adv. Thln Layer Chromatogr. (froc. Sienn. Symp .), 2nd 7980 1982, 483-494. (14F) Sherma, J.; Siellckl, P. J., Jr.; Charvat, S. J. Llq. Chromatogr. 1983, 6, 2679-2685. (15F) Souter, R. W.; Bishara, R. H. J. Ll9. Chromatogr. 1983, 6, 1221-1226. (16F) Srivastava, S. P.; Reena J. Liq. Chromatogr. 1983, 6, 139-143. (17F) Stahr, H. M. J. Liq. Chromatogr. 1984, 7 , 1393-1402. (18F) Thlelemann, H.; Grahnels, H. Z.Gesamte Wg. Ihre Grenzbeg. 1983, 2 9 , 374-375. Chem. Abstr. 1983, 9 9 , 156941n. (19F) Van den Heede, M.; Cordonnler, J.; Van Bever, L.; Heyndrlckx, A. MededFac. Landdbouwnet., Rvksunlv. Gent 1982, 47, 421-434. Chem. Abstr. 1983, 9 8 , 48083e. (20F) Vltorovic, S. L. ”Pestic. Chem.: Hum. Welfare Environ., Proc. Int. Congr. Pestic. Chem., 5th 1982”; Pergamon: Oxford, U.K., 1983; Vol. 4. pp 101-104. (21F) Wood, A. B.; Kanagasabapathy, L. festic. Scl. (Engl.) 1983, 74, 108-118. (22F) Zakarla, M.; Gonnord, M. F.; Gulochon, G. J. Chmmatogr. 1983, 271; Chromatogr. Rev, 2 7 , 127-192. MISCELLANEOUSTECHNfOUES (1G) Bartels, H.; Walser, P. Fresenius’ Z.Anal. Chem. 1983, 375, 6-11. (2G) Behadikova, H.; Popl, M.; Jakublckova, V. Collect. Czech. Chem. Commun. 1983, 48, 2636-2643. Chem. Abstr. 1984, 100, 19140a. (3G) Blaha, J. J.; Ready, DuWayne, E.; Meloan, C. E.; Ohno, M. Anal. Chem. 1984, 5 6 , 845-847. (40) Bostlck, W. D.; Denton, M. S.; Dinsmore, S. R. Report 1983, EPRI-CS2828, Available from NTIS No. DE 83007425, 66 pp. (50) Brattaln, R. L.; Fay, P. K.; Lockerman, R. H. Agron. J. 1983, 75, 192-1 94 - . (6G) Casterllne, J. L., Jr.; Bradlaw, J. A.; Puma, B. J. J. Assoc. Off. Anal. Chem. 1983, 66, 1138-1139. (7G) Durand, P.; Nlcaud, J. M.; Mallevialle, J. J. Anal. Toxlcol. 1984, 8 , 112-1 17. (8G) Goldberg, M. C. Scl. TotalEnvlron. 1982, 2 4 , 73-84. (9G) Greenhalgh, R.; Blackwell, B. A.; Preston, C. M.; Murray, W. J. J. Agric. Food Chem. 1983, 3 1 , 710-713. (100) Horvath, L. Report 1982, IAEAR-1793-F, 8 pp. (Avail. from INIS). (110) Kanlansky, D.; Madajova. V.; Hutta, M.; Zikova, I. J. Chromatogr. 1984, 286, 395-408. (120) Kannangara, T.; Slmpson, G. M.; Rajkumar, K.; Murphy, 8. D. J. Chromatogr. 1984, 283, 425-430. (13G) Kirkbright, G. F.; Shaw, A. E. S. Can. J. Spectrosc. 1983, 2 8 , 100- 103. (140) Knopp, D.; Nuhn, P. Zentralbl. fharm. pharmakother. Laboratorlumsdlagn. 1983, 122, 177. Anal. Abstr. 1983, 45. 3G30. (15G) Lam, N. K.; Kopanica, M. Anal. Chim. Acta 1084, 767, 315-324. (l6G) Manem, J.; Mallevialle, J.; Durant. P.; Chabert, E. Eau, Ind. Nuisances 1983, 74, 31-34. Chem. Abstr. 1983, 9 9 , 75947s. (170) Mazzola. E. P.; Borsetti. A. P.; Page, S. W.; Bristol, D. W. J. Agric. FoodChem. 1984, 3 2 , 1102-1103. (18G) Melghen. E. A.; Slessor, K. N.; Grant, 0. 0. J. Chem. Ecol. 1082, 8, 911-921. (19G) Schwalbe, M.; Dorn, E.; Beyermann, K. J. Agric. Food Chem. 1984, 3 2 , 734-741, (20G) Shushan, B.; Fulford, J. E.; Thomson, 8. A.; Davidson, W. R.; Danylewych, L. M.; Ngo, A.; Nacson, S.; Tanner, S. D. Int. J. Mass Spectrom. Ion f h y s . 1983, 46, 225-228.
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PESTICIDES (210) Stara, V.; Kopanica, M. Collect. Czech. Chem. Commun. 1084, 49, 1282-1288. Chem. Absfr. 1084, 101, 87664s. (22G) Vannelli, J. J.; Schulman, E. M. Anal. Chem. 1084, 56, 1030-1033. (23G) West, S.D.; Dorulla, G. K.; Pooie, G. M. J. Assoc. Off. Anal. Chem. 1083. 66, 111-114.
ORGANOCHLORINEPESTICIDES (1H) Adachl, K.; Ohokunl, N.; Mltsuhashl, T.; Yoshlda, M. J . Assoc. Off. Anal. Chem. 1983, 66, 1315-1318. (2H) Binnemann, P. H.; Sandmeyer, U.; Schmuck, E. 2.Lebensm. Unters. FOrSCh. 1083, 176. 253-261. (3H) Bottomiey, P.; Baker, P. G. Analyst (London) 1084, 109, 85-90. (4H) Brlstol, D. W.; Crlst, H. L.; Lewls, R. G.; MacLecd, K. E.; Sovocool, G. W. J. Anal. Toxlcol. 1082, 6 , 269-275. (5H) British Standards Institution British Standard BS 5666: Part 6: 1983, 10 PP. (6H) Broto-Puig, F Gassiot-Matas, M.; Martinez-Fonrodona, R. J. Efud. Pol/ut. Mar. Medlferr. 6th 1962 1083, 449-454. Chem. Abstr. 1084, 101, 157348w . (7H) Buchholz, H.; Bassler, R; Janssen, E. Landwirtsch. Forsch. 1083, 36, 151-160. Chem. Absfr. 1084, 100, 66692s. (8H) Bush, B.; Snow, J. T.; Connor, S. J. Asqoc. Off. Anal. Chem. 1083, 66, 248-255. (9H) Bush, 8.; Barnard, E. L. Aoal. Lett. 1982, $5,1643-1648. (IOH) Bushway, R. J.; Bureau, J. L.; AiJerayed. A. J . Llq. Chromafogr.
iaad., 7 , 1185-1193
(1IH) Carr, R. S.; Thomas, P.; Neff, J. M. Bull. Envlron. Contam. Toxicol. 1982, 26, 477-479. (12i-t) Contardi, V.; Capeiii, R.; Zanicchi, G.; Drago, M. Analyst (London) 1083, 108, 510-514. (13H) Drummond, I.; Van Roosmalen, P. B.; Kornlcki, M. Inf. Arch. Occup. EflVirOfl.Health 1982, 50, 321-327. (14H) Elakovich, S. D. Bull. Envlron. Confam. Toxlcol. 1982, 29, 489-475. (15H) Erney, D. R. J. Assoc. Off. Anal. Chem. 1083, 66, 969-973. (16H) Fan, De Fang; Ge, Shin Ding J. Assoc. Off. Anal. Chem. 1082, 65, 1517-1520. (17H) Fullerton, F. R.; Oller, W. J.; Biliedeau, S. M.; Everett, G. W. J. Agrlc. FoodChem. 1082, 30, 1117-1119. (18H) Garcia-Gutlerrez,A.; McIntyre, A. E.; Lester, J. N.; Perry, R. Environ. Technol. Lett. 1083, 4 , 129-140. (19H) Garcia-Gutlerrez, A.; McIntyre, A. E.; Lester, J. N. Environ. Technol. Lett. 1082, 3 , 541-544. (20H) Harz, A.; Muelder, U. Lebensmittelchem. Gerlchfl. Chem. 1083, 37, 146-147. Chem. Absfr. 1084, 101, 5594k. (21H) Hunter, K. J . Chromafogr. 1084, 299, 405-414. (22H) Jansson, B.; Wldeqvist, U. Inf. J. Environ. Anal. Chem. 1983, 13, 309-321. (23H) Karanth, N. G. K.; Srimathl, M. S.; Majumder, S. K. J. Envlron. Scl. Health, Part B 1083, B I B , 745-755. (24H) Kline, W. F.; Alien, C. F.; Chester, S. N.; Hiipert, L. R.; Wise, S. A. NBS Speclalfubl. 1983, 656, 91-97. (25H) Kobayashi, H.; Sato, K.; Matano, 0.; Goto. S. Nlppon Noyaku Gakkaishi 1983, 8 , 105-110. Chem. Absfr. 1083, 99, 100820e. (26H) Kongovl, R. Am. Lab. 1984, 76 ( 2 ) ,128-135. (27H) Kotarskl, A. Pesflc.-CIfAC Methods Proc. Ser. 1981, 3 , 131-135. (28H) Lamour, M. Mater. Org. 1082, 17, 67-79. Anal. Absfr. 1083, 45(1), 1C98. (29H) Mayfieid, R. J.; Russell, I.M. Analyst (London) 1083, 108, 322-328. (30H) McMurtrey, K. D.; Holcomb, A. E.; Ekwenchi, A. U.; Fawcett, N. C. J. Llq. Chromatogr. 1084, 7 , 953-960. (31H) Meemken, H. A,; Fuerst, P.; Habersaat, K. Dfsch. Lebensm.-Rundsch. 1982, 78, 282-287. Anal. Absfr. 1083, 44, 2G18. (32H) Noren, K. Arch. Envlron. Contam. Toxicol. 1083, 12, 277-283. (338) Opelanio, L. R.; Rack, E. P.; Blotcky, A. J.; Crow, F. W. Anal. Chem. 1983, 55, 677-681. (34H) Parlar, H.; Kotzlas, D.; Korte, F. Chemosphere 1983, 12, 1453-1458. (35H) Pfannhauser, W.; Thailer, A. Dfsch. febensm.-Rundsch. 1082, 78, 124-125. Anal. Absfr. 1082, 43, 5F18. (36H) Ribick, M. A,; Zajicek, J. Chemosphere 1083, 12. 1229-1242. (371-1) Sawyer, L. D. J. ASSOC.Off. Anal. Chem. 1082, 65, 1122-1128. (38H) Stein, V. B.; Narang, R. S. J . Assoc. Off. Anal. Chem. 1084, 67, 111-116. (39H) Stijve, T. fesflc Chem .: Hum. Welfare Envlron Roc. Inf congr fesflc. Chem., 5th 1982 1983, 4 , 95-100. (40H) Szymczynski, G. A,; Waliszewskl, S. M. J . Androl. 1082, 3 , 149-150. Anal. Absfr. 1083, 4 4 , 4D143. (41H) Takel, G. H.: Kauahlkaua. S. M.; Leong, G. H. Bull. Environ. Contam. ‘ Toxicol. 1983, 30, 606-613. (42H) Thielemann, H. 2.Oesamfe /-!vg. Ihre Grenzgeb. 1983, 29, 267-268. Chem. Abstr. 1983, 99, 110436~. 143H) Venant. A.: Borrel. S.: Richou-Bac, L. Analusis 1082, 10, 333-335. ’ Chem. Absfr. 1983, 98, 15542a. (44H) Waliszewskl, S. M.; Szymczynskl, G. A. Arch, Envlron. Contam. Toxicol. 1083. 12, 577-580. (45H) Wegman, R. C. C.; Hofstee, A. W. M. Water Res. 1982, 16, 1265- 1272. (46H) Wheeler, W. 8.; Thompson, N. P.; Edelsteln, R. L.; Littell, R. C.; Krause, R. T. J. Assoc. Off. Anal. Chem. 1082. 65,1112-1117. (47H) Young, S.; Clower, M., Jr.; Roach, J. A. G. J. Assoc. Off. Anal. Chem. 1084, 67, 95-106.
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ORaANOPHOSPHORUS PESTICIDES (11) Adachi, K.; Ohokuni, N.; Mitsuhashi, T. J. Assoc. Off. Anal. Chem. 1084, 67, 798-800. (21) Alawi, M. A. Fresenlus’ Z . Anal. Chem. 1983, 315, 358-359.
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APRIL 1985
(31) Bhaskar, S. U.; Nandakumar, N. V. J. Assoc. Off. Anal. Chem. 1982. 65, 1297-1298. (41) Bhaskar, S. U.; Nandakumar, N. V.; Raju, G. S.; Visweswaraiah, K.; Majumder, S. K. J. FoodScl. Technol. 1982, 19, 127-128. (51) Cairns, T.; Slegmund, E. 0.; Bong, R. L. Anal. Chem. 1084, 56, 2547-2552 (6I)-ChanTc. T. F.; Crowley, R. J.; Geyer, R. J. Forensic Scl. 1083, 28, 122- 127. (71) Department of the Envlronment and National Water Council (UK) Methods Exam. Wafers Assoc. Mater, 1083, 18 pp. (81) Donseiffen,J. W.; Verwaal, W. festlc. Chem.: Hum. Welfare Envlron., froc. Inf. Congr. Pestic. Chem., 5th 1982 1083, 4 , 105-110. (91) Drescher, W.; Fiedler, L. Chemosphere 1083, 12. 1605-1610. (101) Drevenkar, V.; Froebe, Z.; Stengl, 8.; Stefanac, Z. Anal. Chim. Acta 1983, 154, 277-286. (111) Drevenkar, V.; Stengl, 8.; Tkalcevic, B.; Vasiilc, 2. Inf. J. Envlron. Anal. Chem. 1083, 14, 215-230. (131) Haniff, I. M.; Zienius, R. H. J. Chromafogr. 1983, 264, 33-46. (141) Haniff, I. M.; Zienius, R. H. J. Chromafogr. Scl. 1083, 21, 154-160. (151) Hattori, H.; Suzukl, 0.; Yasuoka, T.; Asano, M.; Katsumata, Y. Nlppon Hoigaku Zasshl 1082, 36, 411-413. Anal. Absfr. 1989, 45, 2D106. (161) Hili, A. R. C.; Wllkins, J. P. G.; Findlay, N. R. I.; Lontay, D. E. M. Analyst (London) 1084, 109, 483-487. (171) Kadam, A. N.; Qhatge, B. B. fesffckfes1084, 18, 20-21. Chem. Absfr. 1084, 101, 67661~. (181) Katlha, S. M.; Nath, A. Indlan J. Agrlc. Scl1082, 52, 549-550. (191) Krause, R. T.; Mln, Z.; Shotkin, S. H. J. Assoc. Off. Anal. Chem. 1983, 66, 1353-1357. (201) Lehmann, R. G.; Smith, L. M.; Wiedmeyer, R. H.; Petty, J. D, J. Assoc. Off. Anal. Chem. 1083, 66, 673-676. (211) Liebowltz, D. P.; Kriz, J. A. Am. Ind. Hyg. Assoc. J. IOBS, 4 4 , 567-571. (221) Lin, S.-N.; Caprlolt, R. M.; Murphy, S. 0. J. A@. FoodChem. 1083, 31, 756-759. (231) Lubs, M.; Hamann, J.; Heeschen, W. Mllchwlssenschaft 1083, 38, 597-600. Chem. Abstr. 1084, 100, 4888v. (241) Mlchalke, P. Benr. Gerlchf. Med. 1983, 4 1 , 103-107. Chem. Abstr. 1983, 99, 207499j. (251) Michaike, P. 2.Rechtsmed. 1982, 68, 195-202. Anal. Absfr. 1083, 4 4 , 5D95. (281) Mirashi, S. V.; Kurhekar, M. P.; D’Souza, F. D.; Meghal, S. K. J. Chromafogr. 1083, 268, 352-354. (271) Neicheva, A.; Vaslleva-Aleksandrova, P.; Kovacheva, E. Mikrochim Acta 1984, 1, 393-398. (281) Ott, D. E.; Gunther, F. A. J. Assoc. Off. Anal. Chem. 1083, 66, 108-1 IO. (291) Petzlnger, 0.; Barry, T. L.; Stenson, M. Bun. Environ. Confam. Toxicol. 1983, 31, 116-119. (301) Sonobe, H.; Carver, R. A.; Krause, R. T.; Kamps, LaVerne R. J. Agrlc. Food Chem. 1082, 30, 696-702. (311) Stan, H. J.; Kellner, G. Biomed. Mass. Specfrom. 1082, 9 , 483-492. (321) Stijve, T. Spec. fubl. RoyalSoc. Chem. 1984, 49, 293-302. Chem. Absfr. 1084, 101, 534453. (331) Sultatos, L. G.; Costa, L. G.; Murphy, S. D. Chromatographla 1982, 15, 669-67 1. (341) Szeto, S. Y.; Brown, M. J. J. Agrlc. Food Chem. 1082, 30, 1082- 1086. (351) Thompson, C. M.; Nishloka, T.; Fukuto, T. R. J. Agric. Food Chem. 1983, 31, 696-700. (361) White, K. D.; Min, Z.; Brumley, W. C.; Krause, R. T.; Sphon, J. A. J. Assoc. Off. Anal. Chem. 1083, 66, 1358-1364.
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CARBAMATE PESTICIDES (IJ) Aicock, N. J.; Corbelli, L.; Games, D. E.; Lant, M. S.; Westwood, S. A. Blomed. Mass Spectrom. 1082, 9 , 499-504. (2J) Aleksandrova, L. 0.; Klisenko, M. A. J. Chromatogr. 1982, 247, 255-262. (3J)Appaiah, K. M.; Kapw, 0.; Nagaraja, K. V. J. Assoc. Off. Anal. Chem. 1083, 66, 105-107. (4J) Bahig, M. E.; Schmidt, E. Isof. Radlaf. Res. 1082, 14, 43-48. (5J) Bayoumi, 0. C.; Galoux, M.; Bernes, A. Meded. Fac. Landbouwwef.. Ruksuniv. Gent 1983, 48, 997-1005. (6J) Cairns, T.; Siegmund, E. G.; Doose, G. M. Biomed. Mass Specfrom. 1083, 10, 24-29; (7J) Cairns, T.; Siegmund, E. G.; Doose, G. M. Bull. Environ. Contam. Toxlc O ~ .1083, 30, 93-98. (a)Cairns, T.; Siegmund, E. G.; Doose, G. M.; Langham, W. S.; Chiu, K. S. Bull. Envlron. Contam. Toxicol. 1084, 32, 310-315. (9J) Calrns, T.; Siegmund, E. 0.;Stamp, J. J. Blomed. Mass Spectrom. 1084, 1 1 , 301-307. (1OJ) DeBerardlnls, M., Jr.; Wargin, W. A. J. Chromabgr. 1082, 246, 89-94. ( I IJ) Dekker, A.; H~ux,N. W. H. J. Envlron. Scl. Heanh, Parf B 1083, B I B , 379-392. (12J) De Kok, A.; Vos, Y. J.; Van Garderen. C.; De Jong, T.; Van Ogstal, M.; Frel. R. W.: Geerdink, R. M.; Brinkman, U. A. T. J . Chromafogr. 1084, 288, 71-89. (la)Draper, W. M.; Lucero, C. M.; Street, J. C. J. Agric. Food Chem. 1982, 30, 1002-1004. ll4Jl Grou. E.: Radulescu. V.: Csuma. A. J. Chromafogr. 1083, 260, ‘ 502-506.‘ 115J) Guhlmann, A,: Hollweg, J.; Seqhofer, F. Beifr. Tabakforsch. Inf. 1983, . 12. 87-91. Anal. Abst?. 1084, 46, 3G20. (16J) Hargreaves, P. A.; Melksham, K. J. Pesflc. Scl. 1083, 14, 347-353. (17J) Hill, K. M.; Hollowell, R. H.; Dal Cortivo, L. A. Anal. Chem. 1984, 56, 2465-2468.
PESTICIDES
(l8J) Hitchman, M. L.; Ramanathan, S. Anal. Chlm. Acta 1084, 157, 349-354. (19J) Hyde, W.; Stahr, H. M.; Moore, R.; Domoto, M.; Pfelffer, R. A&. Thin Layer Chromatogr., [Proc. Blenn. Symp.], 2nd 1980 108b 439-450. Edited by Touchstone, J. C.; Wiley: New York, NY. (20J) Inman, R. D.; Kilgemagl, U.; Delnzer, M. L. J . Agric. Food Chem. 1083. 31. 918-919. (21J) Inman, R. D.; Kllpmagl, U.; Griffin, D. A.; Delnzer, M. L. J. Agrlc. Food Chem. 1083. 31. 722-726. (22J) Kossmann, A.; Ebing, W. Nachrlchtenbl. Dtsch. Pf/anzenschutzdlenstes (Braunschweig)1084, 36, 36-39. Chem. Abstr. lP84, 101, 109054a. (23J) Krause, R. T.; August, E. M. J. ASSOC.Off. 4pal. Chem. 1083, 66, 234-240. (24J) Kumar, Y. J . Enulron. Sol. Health, fartB 1083, 618. 757-765. (25J) Lauren, D. R. J. Assoc. Off. Anal. Chem. 1084, 67, 655-657. (26J) Lauren, b. R.; Agnew, M. P. J . Chromatogr. 1084, 292, 439-443. (27J) Lee, Y. W.: Westcott, N. D. J . Agrlc. Food Chem. 1083, 8 1 , 92-96. (28J) Leppert, B. C.; Cllck, J. C.; Burt, J. E. J . Agric. Foodchem. 1084, 32, 1441. (29J) Leppert, B. C.; Markie, J. C.; Heit, R. C.; Fujle, G. H. J . Agrlc. Food Chem. 1043, 3 7 , 220-223. (3OJ) Miles, C. J.; Delflno, J. J. J . Chromatogr. 1084, 299, 275-280. (315) Muszkat, Lea; Aharonson, N. J . Chromatogr. Scl. 1083, 2 1 , 41 1-414. (32J) Narang, A. S.; Eadon, 0. Int. J. Envlron. Anal. Chem. 1082, 1 1 , 167- 174. (33J) Neisen, T. R.; Cook, R. F.; Gruenauer, M. H.; Gilbert, M. D.; Wltkonton, S. J. Agrlc. FoodChem. 1083, 3 1 , 1147-1150. (34J) Nondek, L.; Frel, R. W.; Brinkman, U. A. T. J . Chromafogr. 1083, 282, 14I150. (35J) Oglerman, L. J. Assoc. Off. Anal. Chem. 1082, 6 5 , 1452-1456. (36J) Oglerman, L. Pestlc. Sci. 1083, 14, 417-422. (37J) She, L. K.; Brlnkman, U. A. T.; Prei, R. W. Anal. Lett. 1084, 17, 915-931. (38J) Spalk, J.; Janauer, G. E.; Lau, M.; Lemley, A. T. J. Chromatog. 1082. 253, 289-294. (39J) Splttler, T. D.;Maraflotl, R. A. J . Chromatogr. 1083, 255, 191-198. (40J) Szeto, S. Y.; Wilkinson, A. T. S.; Brown, M. J. J. Agrlc. FoodUhem. im. .- - ., 32 - - , 78-80 . - - -. (41J) Trehy, M. L.; Yost, R. A.; McCreary, J. J. Anal. Chem. 1064, 5 6 , 1284-1285. (42Jf-Wrlght; L. H.; Jackson, M. 0.; Lewls, R. G. Bull. Envlron. Contam. TOXlCOl. 1082, 28. 740-747. (43J) Wueest, 0.; Meler, W. Z . Lebensm.-Unters.-Forsch. 1083, 177. 25-29. ( 4 4 ) Zhong, W. 2.; Lemley, A. T.; Spallk, J. J . Chromatogr. 1084, 299, 269-274. HERBICIDES AND PLANT QROWH REQULATORS
(IK) Aakerblom, M.; Alex. 0. J . Assoc. Off. Anal. Chem. 1084, 6 7 , 853-655. (2K) Ahmad, I . J. Assoc. Off. Anal. Chem. 1883, 86, 663-666. (3K) Ahmad, I. J. Envlron. Scl. Health, f # r t B 1083, 6 1 8 , 207-219. (4K) Alawl, M. A. Fresenius' Z . Anal. Chem. 1082, 312, 536-538. (5K) Albery, W. J.; Fleet, B.; Brett, A. M. 0. J. Appi. Electrochem. 1084. 14, 550-553. (6K) Allen, J. R. F.; Rlvler, L.; Pllet, P. E. fhyfochemistry 1082, 2 1 , 525-530. (7K) Allender, W. J. J . Anal. Toxlcol. 1083. 7 , 79-82. (8K) Archer, T. E.; Stokes, J. D. J. Agric. FoodChem. 1083, 3 1 , 286-288. (9K) Balm, M. A.; Hill, H. H., Jr. J . Chromatogr. 1083, 279, 631-642. (10K) Bardalaye, P. C.; Wheeler, W. B. Analyst (London) 1084, 109, 255-258. (11K) Grdalaye, P. C.; Wheeler, W. B. J . Assoc. Off. Anal. Chem. 1084, 67,280-284. (12K) Bardalaye, P. C.; Wheeler, W. 6.; Templeton, J. L. J . Assoc. Off. Anal. Chem. 1084, 6 7 , 904-909. (13K) Biakesley, D.; Hall, J. F.; Weston, G. D.; Elllott, M. C. J . Chromatogr. 1083. 258. 155-164. (14K) Bouchard, D. C.; Lavy, T. L. J . Chromatogr. 1083, 270, 396-401. (15K) Brinkman, U. A. T.; De Kok, A.; Geerdlnk, R. B. J . Chromafogr. lB84, 283, 113-126. (16K) Brown, D. F.; McDonough, L. M.; McCool, D. K.; Papendlck, R. I. J . Agrlc. Food Chem. 1084, 3 2 , 195-200. (17K) Buchberger, W.; Mallssa, H.; Wlnsauer, K. Mlkrochlm. Acta 1084, I , 53-61. (18K) Cairns, T.; Slegmund, E. G.; Doose, 0. M. Bull. Envlron. Contam. TOXICOll.1083, 30, 234-236. (l9K) Cessna, A. J. Agr/c. FoodChem. 1084, 3 2 , 171-173. (20K) Connlck, W. J., Jr.; Bradow, J. M. J. Agrlc. Food Chem. 1084, 32. 200-202. (21K) &k, A. M.; Bellstein, P.; Huetter, R. Int. J. Envlron. Anal. Chem. 1083. 14. 93-98. (22K) Deleu, R.; Copln, A. HRC CC, J. Hlgh Resold. Chromatogr. Chromatogr. Commun. 1082, 5 , 682-883. (23K) Dumbroff, E. 6.; Walker, M. A.; Dumbroff, P. A. J . Chromatogr. 1083, 256, 439-446. (24K) Frankenberger, W. T., Jr.; Brunner, W. SoilScl. Soc. Am. J . 1083, 47, 237-241. (25K) Oeloux, M.; Van Damme, J. C.; Bernes, A. J. Chromatogr. 1082. 242, 323-330. ._. .._ (26K) Oeloux, M.; Van Damme, J. C.; Bernes, A. J. Assoc. Off. Anal. Chem. 1082, 65, 24-27. (27K) (3111, R.; Qua. S. C.; Moffat, A. C. J. Chromatogr. 1083, 255, 463-490.
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PESTICIDES (83K) Wells, M. J. M.; Michael, J. L.; Neary, D. G. Arch. Envlron. Contam. TOX~COI.1984, 13, 231-235. (84K) Wong, Y.4. J. Assoc. Off. Anal. Chem. 1982, 6 5 , 1118-1121. (85K) Worobey, B. L. J. Chromatogr. 1983,262, 328-330. (86K) Worobey, B. L.; Panopio, L. 0. Anal. Lett. 1983, 16, 1235-1252. (87K) Wurst, M.; Prlkryl, 2.; Vokoun, J. J. Chromatogr. 1984, 286, 237-245. (88K) Yamaguchi, I.; Fujlsawa, S.;Takahashi, N. Phytochemistry 1982,2 1 , 2049-2055. (89K) You, LS.;Bartha, R. J. Agric. FoodChem. 1982, 30, 1143-1147. (90K) Young, C. C. Proc. Nati. Sci. Counc., Repub. China, Part 8 1984,8 , 119-123. Chem. Abstr. 1984, 101, 205919g. (91K) Zahnow, E. W. J. Agrlc. Food Chem. 1982,3 0 , 854-857. (92K) Zahnow, E. W. J. Agric. FoodChem. 1984,3 2 , 953.
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(7M) Jiang, M.; Soderlund, D. M. J. Chromatogr. 1982,248, 143-149. (8M) McCown, S. M. L . LC, Liq. Chromatogr. HPLC Mag. 1984, 2 , 804-806. (OM) Nlkiforov, A,; Kohlmann, H. Int. J. Mass Spectrom. Ion Phys. 1983, 48, 141-144. (10M) Oi, N.; Nagase, M.; Inda, Y.; Doi, T. J. Chromatogr. 1983, 259, 487-493. (11M) Otieno, D. A.; Jondiko, I. J.; McDowell, P. G.; Kezdy, F. J. J. Chromatoar. Sci. 1982. 2 0 . 566-570. 12Mi Page, C. T.; Thomas, C. Commun.-Wool Res. Organ. N. Z.,C80, I983 p 20. Anal. Abstr. 1984,46, 4C88. 13M) Papadopoulou-Mourkldou,E. Residue Rev. 1983,8 9 , 179-208. 14M) Papadopoulou-Mourkldou, E.; Iwata, Y.; Gunther, F. A. J. Agrlc. Food Chem. 1984,32, 800-805. 15M) Papadopoulou-Mourkidou,E.; Iwata, Y.; Gunther, F. A. J . Agric. Food Chem. 1983,3 1 , 629-633. 16M) Richard, A.; Andermann, G. J. Chromatogr. Scl. 1984, 2 2 , 207-210. 17M) Schoor, W. P.; McKenney, C. L., Jr. Bull. Environ. Contam. Toxlcol. 1983,3 0 , 84-92. 18M) Sedea, L.; Tonlnelli, G.; Sartorel, B. Riv. Ital. Sonstanze Grasse 1983, 60, 133-137. Chem. Abstr. 1984, 100, 116315~. 19M) Slebers, J.; Nolting, H. G. Nachrlchtenbl. Dtsch. Pflanzenschutzdienstes (Braunschweig) 1082, 3 4 , 166-170. Anal. Abstr. 1982, 43, 5G41. (20M) Smith, S.;Willis, G. H.; McDowell, L. L. J. Agric. Food Chem. 1983, 3 1 , 610-612. (21M) Spittler, T. D.; Argauer, R. J.; Lisk, D. J.; Mumma, R. 0.; Wlnnett, G.; Ferro, D. N. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 824-826. (22M) Sundararajan, R.; Chawla. R. P. J. Assoc. Off. Anal. Chem. 1983, 66, 1009-1012.
FUMIGANTS (1N) Collins, M.; Barker, M. J. Int. Lab. 1983, 1 3 ( 7 ) ,106, 108, 110-112, 114-116. (2N) Chang, L. T. F.;Crowley, R. J.; Delliou, D.; Geyer, R. J. Anal. Toxlcol. 1983, 7,185-187. (3N) Daft, J. L. J. Assoc. Off. Anal. Chem. 1983, 66, 228-233. (4N) Dumas, T.; Bond, E. J. J. Assoc. Off. Anal. Chem. 1982, 65, 1379-1381. (5N) Iwata, Y.; Duesch. M. E.; Gunther, F. A. J. Agric. FoodChem. 1983, 3 1 , 171-174. (6N) Kastl, P. E.; Hermann, E. A. J. Chromatogr. 1983. 265, 277-283. (7N) Leiber, M. A.; Berk, H. C. Anal. Chem. 1984,5 6 , 2134-2137. (8N) Morris, S. C.; Rlppon, L. E.; Halamek, R. J. Chromatogr. 1982, 246, 136-140. (9N) Nazer, I . K.; Hallak, A. B. Abu-Gharbleh, W. I.; Saleh, N. S.J. Radloanal. Chem. 1982, 7 4 , 113-116. (ION) Rangaswamy, J. R. J. Assoc. Off. Anal. Chem. 1984,67, 117-122.
MISCELLANEOUS PEST1CI DES (1P) Addison, J. B. J. Assoc. Off. Anal. Chem. 1982, 6 5 , 1299-1301. (2P) Adler, I.L.; Hofmann, C. K.; Stavinski, S. S. J. Agrlc. Food Chem. 1984,3 2 , 1358-1361. (3P) Daharu, P. A.; Sporns, P. J. Agrlc. FoodChem. 1984,32, 108-111. (4P) Dawson, V. K. Can. J. Fish. Aquat. Scl. 1982,3 9 , 778-782. (5P) Dawson, V. K.; Harman, P. D.; Schultz, D. P.; Allen, J. L. Trans. Am. Fish. SOC. 1983, 112, 725-727. (6P) Feng, C. C.; Sundaram, K. M. S.J. Li9. Chromatogr. 1984,7 , 95-109. (7P) Glardl, M. T.; Giardlna, M. C.; Brancaleonl, E. Anal. Chem. Symp Ser. 1083, 13, 53-61. (%P) Haefner, M. Gesunde, Pflanz, 1983, 3 5 , 177-188. Chem. Abstr. 1983,9 9 , 135377t. (9P) Hobson-Frohock, A. Analyst (London) 1982, 107, 1195-1 199. (1OP) Hoogenboom, J. J. L.; Rammell, C. G. Bull. Environ. Contam. Toxicol. 1983,31, 239-243. (11P) Hornish, R. E.; Clasby, M. A,; Nappier, J. L.; Nappler, J. M.; Hoffman, G. A. J. Agric. Food Chem. 1984,3 2 , 1219-1223. (12P) Hunter, K. J. Chromatogr. 1983,270, 267-276. (13P) Hunter, K. J. Chromatogr. 1983,270, 277-283. (14P) Inoue, M.; Hagimoto, T. Nippon Noyaku Gakkaishi 1983,8 , 321-328. Chem. Abstr. 1984, 100, 1 1 6 3 1 7 ~ . (15P) Lee, H. B.; Chau, A. S. Y. J. Assoc. Off. Anal. Chem. 1983, 66, 1029-1 038. (16P) Lee, H. B.; Weng, L. D.; Chau, A. S.Y. J. Assoc. Off. Anal. Chem. 1984,6 7 , 789-794. (17P) Li, Y. C.; Strupp, D.; Kossmann, A.; Ebing, W. Fresenius’ 2. Anal. Chem. 1983,376, 290-292. (18P) McCown, S.M. LC, Liq. Chromatogr. HPLC Mag. 1983. 1, 586-567. (19P) McCown, S.M. LC,Llq. Chromatogr. HPLCMag. 1984,2, 318-319. (20P) Moellhoff, E. Pflanzenschutz .-Nachr. 1983, 36, 54-62. Chem. Abstr. 1984, 101, 124710e. (21P) Odanaka, Y.; Tsuchiya. N.; Matano, 0.; Goto, S. Anal. Chem. 1983, 5 5 , 929-932. (22P) Pflugmacher. J.; Eblng, W. 2.Lebensm .-Unters.-Forsch. 1984, 178, 90-92, Anal. Abstr. 1984,46, 9G23. (23P) Shiga, N.; Matano, 0.; Goto. S.J. Chromatogr. 1983,257, 151-156.
.
PYRETHROIDS
INDUSTRIAL CHEMICALS RELATEDTO PESTICIDES
(1M) Akhtar, M. H. J. Chromatogr. 1982,246, 81-87. (2M) Bolygo, E.; Zakar, F. J. Assoc. Off. Anal. Chem. 1983, 66, 1013-1017. (3M) Chapman, R. A. J. Chromatogr. 1983,258, 175-182. (4M) David, D. Bull. Envlron. Contam. Toxlcoi. 1982,2 8 , 733-739. (5M) Dicklnson, C. M. J. Assoc. Off. Anal. Chem. 1982, 6 5 , 921-926. (6M) Grounds, P. R. N . Z.J. Exp. Agric. 1982, 10. 425-428.
Linder, C. E.; Vaz, R. Vaar Foeda 1984, 3 6 , 7-11. (1Q) Anderson, 0.; Chem. Abstr. 1084, 101, 169182a. (2Q) Bankmann, E.; Hotz, R.; Prandi, C.; Sharples, W. G.; Steuerle, H.; Stoerl, M.; Weis, H.; Zatka, A. Chemosphere 1884, 13, 499-508. (3Q) Becker. D. A. NBS Spec. Pubi. (U. S.) 1984,No. 674, 33-41. (40) Burse, V. W.; Needham, L. L.; KOrver, M. P.; Lapeza, C. R., Jr.; Liddle, J. A.; Bayse, D. D. J. Assoc. Off. Anal. Chem. 1983,66, 32-39.
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ANALYTICAL CHEMISTRY, VOL.
57, NO. 5, APRIL 1985
Anal. Chem. 1985, 57, 15R-29R (5Q) Burse, V. W.; Needham, L. L.; Korver, M. P.; Lapeza, C. R., Jr.; Llddle, J. A.; Bayse, D. D. J. Assoc. Off. Anal. Chem. 1983, 6 6 , 40-45. (6Q) Buser, H. R.; Rappe, C. Anal. Chem. 1984. 5 6 , 442-448. (7Q) Cochrane, W. P.; Miles, W.; Wakeford, B.; Slngh, J. Pestlc. Chem.: Hum. Welfare Envlron., Proc. Int. Pestlc. Chem. 5th 7982 1983, 4 , 341-348. Edited by Mlyamoto, J.; Kearney, P. C.; Pergamon, Oxford, UK. (80) De Kok, A.; Qeerdlnk, R. 6.; De Vrles, G.; Brlnkman, U. A. T. Int. J. Envlron. Anal. Chem. 1982, 12, 99-122. (9Q) Duinker, J. C.; Hiliebrand, M. T. J. Bull. Environ. Contam. Toxlcol. . isat, 3 1 , 25-32. (lm)Fawkes, J.; Albro, P. W.; Waiters, D. 6.; McKlnney, J. D. Anal. Chem. 1082, 54, 1866-1871. (IIQ) Gutlerrez, A. G.; McIntyre, A, E.; Lester, J. N.; Perry, R. Envlron. Technol. Lett. 1983, 4 , 521-528. (I2Q) Harless, R. L.; Lewis, R. G.; Dupuy, A. E.; McDanlel, D. D. Envlron. Scl. Res. lg83, 2 6 , 161-171. (13Q) Kennedy, P. A.; Roberts, D. J.; Cooke. M. J. Chromatogr. 1982,249, 257-265. (14Q) Levlne, S. P.; Homsher, M. T.; Sullivan, J. H. J. Chromatogr. 1983, 257, 255-268. (15Q) Lewis, E.; Jamleson, W. D. Int. J. Mass Spectrom. Ion fhys. 1983, 48, 303-306. (I6Q) Llbertl, A.; Clccloll, P.; Brancaieonl, E.; Ceclnato, A. J. Chromatogr. 1982, 242, 111-118. (17Q) Marquez. A. I.€€€ Trans. Power Appar. Syst. 1984, PAS-703 ( 3 ) . 589-592. Chem. Abstr. 1984, 100, 141801g. (l8Q) Mathar, W.; Beck, H. Lebensmlttelchem. Gerlchtl. Chem. 1983, 3 7 , 147-148. Chem. Abstr. 1984, 700,173236t. (l9Q) McKlnney, J. D.; Moore, L.; Prokopetz, A.; Welters, D. B. J. Assoc. Off. Anal. Chem. 1984, 6 7 , 122-129. (20Q) McMurtrey, K. D.: Wlldman, N. J.; Tal, H. Bull. Envlron. Contam. Toxled. 1983, 3 1 , 734-737. (21Q) Mes. J.; Davles, D.; Bryce, F. Int. J. Envlron. Anal. Chem, 1983, 15, 25-37. (22Q) Mlllar, J. D.; Thomas, R. E.; Johnson, D. E. U . S . Envlron. Rot. Agency, Off. Res. Dev., [Rep.] €PA, EPA-80014-82-023, 1982, p 220. (23Q) Mullins, M. D.; Pochlnl, C. M.; McCrlndle, S.;Romkes, M.; Safe, S.H.; Safe, L. M. Environ. Scl. Technol. 1984, 18, 468-476. (24Q) Newton, D. A,; Laskl, R. R. J. Chromatogr. Scl. 1983, 2 1 , 161-185. (25Q) Oehme, M.; Stray, H. Fresenlus' Z . Anal. Chem. 1982, 317, 665-673. (26Q) O'Keefe, P.; Meyer, C.; Dlllon, K. Anal. Chem. 1982, 54, 2623-2625. (27q) Onuska, F. I.; Komlnar, R. J.; Terry, K. A. J. Chromatogr. 1983, 279, 111-1 18. (28Q) Parlar, H.; Mansour, M. Pergamon Ser. Envlron. Scl. 1982, 7 , 241-247.
(29Q) Parris, R. M.; Guenther, F. R.; May, W. E.; Cheder, S. N. NBS Spec. Pub/. ( U . S . ) 1984, NO. 674, 27-32. (30Q) Peakall, D. 6.; Lew, T. S.; Springer, A. M.; Walker, W., 11; Rlsebrough, R. W.; Monk, J. G.; Jarman, W. M.; Walton, B. J.; Reynolds, L. M.; et ai. Arch Envlron. Contam. Toxlcol. 1983, 72, 523-528. (31Q) Pelllzzarl, E. D.; Moseiey, M. A.; Cooper, S. D.; Harry, J. V.; Demlan, 8.; Mullin, M. D. Adv. Exposure, Health Environ. Eff. Stud. PCB's, Symp. PfOC. 1982 1983, (LSI-TR-507-137B, P884-135771), 4-80. Edlted by Davenport, R. J.; Bernard, B. K.; NITS: Sprlngfleld, VA. (32Q) Peters, T. L.; Nestrick, T. J.; Lamparski, L. L. Walter Res. 1984, 18, 1021-1 024. (33Q) Peterson, J. C.; Freeman, D. H. Int. J. Environ. Anal. Chem. 1982, 12, 277-291. (34Q) Rappe. C.; Nygren, M.; Buser, H.; Masuda, Y.; Kuroki, H.; Chen, P. H. Envlron. Scl. Res. 1983, 2 6 , 241-253. (35Q) Russell, D. J.; McDuffle, B. Int. J. Envlron. Anal. Chem. 1983, 15, 185- 183. (36Q) Ryan, J. J.; Pllon, J. C. J . Chromatogr. 1982, 248, 409-415. (37Q) Safe, S.; Parkinson, A.; Robertson, L.; Sayer, T.; Bandlera, S. Report 1983, EPA-600/D-83-098; Order No. PB83-247486, 25 pp. Avail. NTIS, from Gov. Rep. Announce. Index ( U . S . ) 1983, 8 3 , 6058. (38Q) Schulte, E.; Mallsch, R. Fresenlus' 2. Anal. Chem. 1984, 319, 54-59. (39Q) Schwartz, T. R.; Campbell, R. D.; Stalling, D. L.; Little, R. L.; Petty, J. D.; Hogan, J. W.; Kaiser, E. M. Anal. Chem. 1984, 5 6 , 1303-1308. (40Q) Smith, G. C.; Gauger, G. A.; Frey, R. M. I€€€ Trans. Power Appar. Syst., 1982, PAS-101, 2260-2267. Anal. Abstr. 1983, 4 4 , 3C85. (41Q) Smith, R. M.; O'Keefe, P. W.; Hllker, D. R.; Jelus-Tyror, B. L.; Aldous, K. M. Chemosphere 1982, 1 1 , 715-720. (42Q) Splttler, T. M.; Natl. Conf. Manage. Uncontrolled Hazard. Waste Sites 1983, 105-107. Chem. Abstr. 1984, 100, 220890~. (43Q) Stelnwandter, H. Fresenlus' 2.Anal. Chem. 1982, 373, 538-538. (44Q) Stelnwandter, H. Fresenlus' Z . Anal. Chem. 1983, 314, 129-130. (45Q) Stelnwandter, H. Fresenlus' 2. Anal. Chem. 1983, 376, 493-494. (46Q) Takamlya, K. Bull. Environ. Contam. Toxlcol. 1983, 3 0 , 600-605. (47Q) Tulnstra, L. 0. M. T.; Traag, W. A. J. Assoc. Off. Anal. Chem. 1983, 6 6 , 708-717. (48Q) Voyksner, R. D.; Hass, J. R.; Sovocool, G. W.; Bursey, M. M. Anal. Chem. 1983, 55, 744-749. (49Q) Weeraslnghe, N. C. A.; Meehan, J. L.; Gross, M. L.; Galnes, J. J. Agrlc. Food Chem. 1983, 3 1 , 1377-1378. (50Q) Westerberg, R. B.; Allbrando, S. L.; Van Lenten, F. J. J. Chromatogr. 1984, 284, 447-456. (51Q) Wong, A. S. U S . Envlron. Prot. Agency, Off. Res. Dev., [Rep.] EPA-600/4-82-028, 1982 p 51. Anal. Abstr. 1983. 45, 2H107.
Coatings D. G. Anderson* a n d J. T.Vandeberg DeSoto, Inc., 1700 South Mt. Prospect Road, DesPlaines, Illinois 60018
INTRODUCTION This review covers analytical techniques applicable to the examination of coatings and coatings raw materials, substrates upon which coatings are placed, etc., since the last review in 1983 (14). The compiled references were extracted after searching Chemical Abstracts, Analytical Abstracts, World Surface Coatings Abstracts, and the Journal of Coatings Technology. The contents are divided into 18 categories for ready access to the reader. Readers are advised to survey the entire review for the analysis of specific paints, coatings, or related materials may be found in each section. The five most highly referenced categories are Chemical and Electrochemical, Gas Chromatography, Nuclear Magnetic Resonance Spectroscopy, Surface, and Thermal Analysis. New or unique applications to estab!ished analytical techniques also appear throughout this remew. Several general review articles have appeared dealing with the use of analytical techniques for the examination of coatings (1,21,22,23).General analytical papers were also published on more narrow aspects of coatings technology, including emulsion paints (28,311, realistic paint testing (23),and fire retardant coatings (17). The role of ASTM in coatings research and development was the subject of a recent publication (36). Analysis of inks also received special attention (29) as 0003-2700/ 85/0357-15R$06.50/0
did general polymer analysis as detailed in a comprehensive book on this subject (16). The increasing role of the coatings analyst in dealing with customer complaints was the subject of a presentation (15)which cited four examples of how unique analytical approaches are frequently required to reach a resolution to a problem. The examination of coatings for forensic applications has found continued interest during this period (24,30,32)as has the analysis of fine art for conservation purposes (35). Special studies also appeared, including methods of latex cleaning prior to analysis (241, paint solubility testing (36), and a mathematical treatment of methods for calculating the flash point of liquids (34). The American Society for Testing and Materials (ASTM) has continued to provide methods for the examination of coatings. Methods relative to the determination of flash point received special attention, including the use of the Setaflash Tester (9,131, the use of a flash-no flash equilibrium method (ll),and the more traditional Tag cup apparatus (3, 7). ASTM procedures have also dealt with the examination of diatomaceous silica (6) and liquid paint driers (5). Standard practices have also appeared for the testing of specific coatings types, for example, wood furniture lacquers (81, lac resins (2), and clear and pigmented lacquers ( 4 ) were completed during this period. Ultraviolet cured coatings are a new area of @ 1985 American Chemical Society
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