Multiresidue pesticide analysis of wines by dispersive solid-phase extraction and ultrahigh-performance liquid chromatography-tandem mass spectrometry.
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.
Center for Food Safety and Applied Nutrition, HFS-706, US Food and Drug Administration, 5100 Paint Branch Parkway, College Park, Maryland 20740-3835, USA.
Kai
K
Zhang
Jon W
JW
Wong
Douglas G
DG
Hayward
Piyush
P
Sheladia
Alexander J
AJ
Krynitsky
Frank J
FJ
Schenck
Michael G
MG
Webster
Jeffrey A
JA
Ammann
Susan E
SE
Ebeler
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D011786:Quality Control; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014920:Wine / Q000032:analysis*
D010573:Pesticide Residues