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  • Title: Multiresidue pesticide analysis of wines by dispersive solid-phase extraction and ultrahigh-performance liquid chromatography-tandem mass spectrometry.
    Author: Zhang K, Wong JW, Hayward DG, Sheladia P, Krynitsky AJ, Schenck FJ, Webster MG, Ammann JA, Ebeler SE.
    Journal: J Agric Food Chem; 2009 May 27; 57(10):4019-29. PubMed ID: 19371141.
    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 r(2) > 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 (<70%) and higher (>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.
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