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Size Exclusion Chromatographic Cleanup for GC/MS Determination of Organophosphorus Pesticide Residues in Household and Vehicle Dust

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Size exclusion chromatography (SEC) was used as a cleanup method for the analysis of organophosphorus pesticides in household and vehicle dusts. The pesticides investigated were diazinon, methyl parathion, chlorpyrifos, malathion, phosmet, and azinphosmethyl. These compounds are of interest due to their use in agricultural tree fruit production and/or urban pest control. Pesticides were determined via gas chromatography/mass spectrometry with selected-ion monitoring and cool on-column injection. The lower limit of method validation was 0.20 μg/g. Method limits of detection in dust ranged from 0.012–0.055 μg/g. Dust samples were collected with vacuums from the homes and vehicles of people living and working in a rural agricultural region in the central part of Washington State. The analytes were extracted from the dust by sonication in acetone. The extracts were solvent-exchanged to cyclohexane, frozen, thawed, and centrifuged prior to SEC injection. Following SEC, the eluent was split into 2 fractions, concentrated, and injected on-column into the gas chromatograph. This method represents the first complete publication describing the SEC cleanup of organophosphorus pesticides in dusts. Recoveries of pesticides in dusts ranged from 63.5–110.8 ± 4.9–19.6% over a fortification range of 0.20–10.00 μg/g. This optimized, automated, and reproducible SEC method does not require further treatment or cleanup for trace determination of these organophosphorus pesticides.
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Document Type: Research Article

Affiliations: 1: University of Washington, Environmental Health Laboratory, Box 357234, Seattle, WA 98195-7234; SNBL USA, Merrill Cr. Pkwy, Everett, WA 98203. 2: University of Washington, Environmental Health Laboratory, Box 357234, Seattle, WA 98195-7234. 3: University of Washington, Environmental Health Laboratory, Box 357234, Seattle, WA 98195-7234; Oregon Health Sciences University, Center for Research on Occupational and Environmental Toxicology, Portland, OR.

Publication date: January 1, 2002

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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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