Multiresidue Pesticide Analysis of Wines by Dispersive Solid-Phase Extraction and Ultrahigh-Performance Liquid Chromatography−Tandem Mass Spectrometry
- 17 April 2009
- journal article
- Published by American Chemical Society (ACS) in Journal of Agricultural and Food Chemistry
- Vol. 57 (10), 4019-4029
- https://doi.org/10.1021/jf9000023
Abstract
A multiresidue pesticide method is described for the determination of 72 pesticides in wines. Pesticides were extracted using acetonitrile saturated with magnesium sulfate and sodium chloride, followed by solid-phase dispersive cleanup using primary−secondary amine and graphitized carbon black sorbents. Analysis is performed by ultraperformance liquid chromatography−electrospray ionization−tandem mass spectrometry (UPLC-MS/MS). The limits of quantitation (LOQs) for most of the pesticides ranged from 0.3 to 3.3 μg/L with the exception of cyromazine, fenhexamid, and acibenzolar S-methyl (LOQ > 10 μg/L), and quantitation was determined from calibration curves of standards containing 5.0−2500 μg/L with r2 > 0.99. Recovery studies were performed by fortifying wine samples with the pesticides to concentrations of 10, 100, and 1000 μg/L, resulting in recoveries of >80% for most of the pesticides. Lower (120%) recoveries were most likely from complications of pesticide lability or volatility, matrix interference, or inefficient desorption from the solid-phase sorbents. The method was used to analyze 10 wines collected from a market basket survey, and 19 different pesticides, primarily fungicides, were present at concentrations ranging from <1.0 to 1000 μg/L.This publication has 25 references indexed in Scilit:
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