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Optimization of Detection Conditions and Single-Laboratory Validation of a Multiresidue Method for the Determination of 135 Pesticides and 25 Organic Pollutants in Grapes and Wine by Gas Chromatography Time-of-Flight Mass Spectrometry

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This paper describes single-laboratory validation of a multiresidue method for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons, and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC/MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including the temperature-sensitive compounds, like captan and captafol, that are prone to degradation during analysis. An average recovery of 80–120% with RSD <10% could be attained for all analytes except 17, for which the average recoveries were 70–80%. LOQ ranged within 10–50 ng/g, with <25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, the residues of buprofezin, chlorpyriphos, metalaxyl, and myclobutanil were detected, with an RSD of <5% (n= 6); the results were statistically similar to previously reported validated methods.
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Document Type: Research Article

Affiliations: 1: University of Pune, Department of Environmental Sciences, Pune–411 007, India 2: National Research Centre for Grapes, P.O. Manjri Farm, Pune–412 307, India 3: University of Pune, Department of Botany, Pune–411 007, India

Publication date: January 1, 2011

More about this publication?
  • 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 The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better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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