Routine approach to qualitatively screen for 300 pesticides and quantify those frequently detected in fruits and vegetables using liquid chromatography tandem mass spectrometry
Résumé
This paper describes an efficient and effective analytical scheme to first screen for 300 pesticides in fruit and vegetables samples using liquid chromatography tandem mass spectrometry (LC-MS/MS) with a commercial enhanced product ion method, and then presumed positive extracts were analyzed using a quantitative and confirmatory LC-MS/MS method optimized for 55 pesticides. QuEChERS with acetate buffering (AOAC Official Method 2007.01) was used for sample preparation, which has been previously shown to yield high quality results for hundreds of pesticide residues in foods. The advantages and disadvantages of both the qualititative screening and quantitative/confirmatory methods and their combination are critically discussed. No false negatives for the 55 pesticides occurred above 10 ng g-1 for extracts analyzed by both LC-MS/MS methods, and the no false positives were encountered from the screening analysis (after analyst review) because all presumptive identifications were confirmed in the second analysis. The monitoring scheme was applied during a one-year period on 200 fruit and vegetable samples from Hungarian markets. No pesticide residues were found in half of the samples, and 12 violations of European maximum residue limits were determined.
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