Analysis of Pesticide Residues in Mixed Fruit and Vegetable Extracts by Direct Sample Introduction/Gas Chromatography/Tandem Mass Spectrometry

Abstract

Abstract Direct sample introduction (DSI), or “dirty sample injection,” was investigated in the determination of 22 diverse pesticide residues in mixed apple, green bean, and carrot extracts by benchtop gas chromatography/tandem mass spectrometry (DSI/GC/MS–MS). The targeted pesticides, some of which were incurred in the samples, included chlorpyrifos, azinphos-methyl, parathion-methyl, diazinon, terbufos, p,p′-DDE, endosulfan sulfate, carbofuran, carbaryl, propargite, bifenthrin, dacthal, trifluralin, metalaxyl, pendimethalin, atrazine, piperonyl butoxide, diphenylamine, vinclozolin, chlorothalonil, quintozene, and tetrahydrophthalimide (the breakdown product of captan). The analytical DSI method entailed the following steps: (1) blend 30 g sample with 60 mL acetonitrile for 1 min in a centrifuge bottle; (2) add 6 g NaCl and blend 30 s; (3) centrifuge for 1–2 min; (4) add 5 mL upper layer to 1 g anhydrous MgSO4 in a vial; and (5) analyze 11 μL extract, using DSI/GC/MS–MS. Sample cleanup is not needed because GC/MS–MS is exceptionally selective for the targeted analytes, and nonvolatile coextracted matrix components do not contaminate the injector or the GC/MS–MS system. Average recoveries of the pesticides were 103 ± s7% with relative standard deviations of 14 ± 5% on average, and limits of detection were <2 ng/g for nearly all pesticides studied. The DSI/GC/MS–MS approach for targeted pesticides is quantitative, confirmatory, sensitive, selective, rugged, rapid, simple, and inexpensive.