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Multiresidue Method for N-Methyl Carbamates and Metabolite Pesticide Residues at the Parts-per-Billion Level in Selected Representative Commodities of Fruit and Vegetable Crop Groups

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A reversed-phase liquid chromatographic method with both fluorescence and mass spectrometric detection is presented for the determination of 13 parent N-methyl carbamate pesticides and their metabolites, as well as piperonyl butoxide, for a total of 24 compounds in selected fruits and vegetables. The commodities chosen were of special concern to the U.S. Environmental Protection Agency (EPA) because they had the least amount of monitoring data for dietary exposure estimates used in risk assessment. The method is based on a judicious selection of procedures from U.S. Food and Drug Administration sources such as the Pesticide Analytical Manual (Volume I), and Laboratory Information Bulletins, plus additional material from the chemical literature combined in a manner to recover the N-methyl carbamates and their metabolites at the 1 μg/kg or 1 part-per-billion level. The method uses an acetone extraction, followed by an aminopropyl solid-phase extraction cleanup. Determination of residues is by RP-LC, in which the liquid chromatograph is interfaced with either a fluorescence or a mass spectrometric detector. The method is designed so that a set of 6 samples can be prepared in 1 working day for overnight instrumental analysis. Recovery data are presented from analyses of selected commodities in some of EPA's fruit and vegetable crop groupings. A table listing relative retention times is presented for the N-methyl carbamates and their metabolites.
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Document Type: Research Article

Affiliations: 1: U.S. Environmental Protection Agency, Office of Pesticide Programs, Biological and Economic Analysis Division, Analytical Chemistry Branch, Environmental Science Center, 701 Mapes Rd, Mail Code 7503C, Rm C209, Fort George G. Meade, MD 20755-5350. 2: U.S. Food and Drug Administration, Southeast Regional Laboratory, 60 Eighth St NE, Atlanta, GA 30309. 3: U.S. Food and Drug Administration, Center for Food Safety and Applied Nutrition, 5100 Paint Branch Pkwy, College Park, MD 20740-38350. 4: U.S. Environmental Protection Agency, Office of Pesticide Programs, Biological and Economic Analysis Division, Analytical Chemistry Branch, 701 Mapes Rd, Fort George G. Meade, MD 20755-5350; Current address: U.S. Department of Agriculture, 1400 Independence Ave, Washington, DC 20250.

Publication date: 2004-09-01

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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