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Extension of the QuEChERS Method for Pesticide Residues in Cereals to Flaxseeds, Peanuts, and Doughs†

作者:Urairat Koesukwiwat, Steven J. Lehotay, Kateřina Maštovská, Kelly J. Dorweiler, Natchanun Leepipatpiboon · 发表于:Journal of Agricultural and Food Chemistry · 年份:2009 · DOI:10.1021/jf902988b · 被引用次数:204 · 研究领域:Pesticide Residue Analysis and Safety、Analytical Chemistry and Chromatography、Analytical chemistry methods development

A simple method was evaluated for the determination of pesticide residues in flaxseeds, doughs, and peanuts using gas chromatography-time-of-flight mass spectrometry (GC-TOF) for analysis. A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, which was previously optimized for cereal grain samples, was evaluated in these fatty matrices. This extraction method involves first mixing the sample with 1:1 water/acetonitrile for an hour to swell the matrix and permit the salt-out liquid-liquid partitioning step using anhydrous MgSO(4) and NaCl. After shaking and centrifugation, cleanup is done by dispersive solid-phase extraction (d-SPE) using 150 mg of anhydrous MgSO(4), 150 mg of PSA, and 50 mg of C-18 per milliliter of extract. This method gave efficient separation of pesticides from fat and removal of coextracted substances better than gel permeation chromatography or use of a freeze-out step, which involved excessive use of solvent and/or time. The optimized analytical conditions were evaluated in terms of recoveries, reproducibilities, limits of detection, and matrix effects for 34 representative pesticides using different types of flaxseeds, peanuts, and doughs. Use of matrix-matched standards provided acceptable results for most pesticides with overall average recoveries between 70 and 120% and consistent RSDs <20% for semipolar pesticides and <26% for lipophilic pesticides. The recoveries of these latter types of pesticides depended on the fat conte...