title: Optimization of two-dimensional gas chromatography time-of-flight mass spectrometry for separation and estimation of the residues of 160 pesticides and 25 persistent organic pollutants in grape and wine.
abstract: Two-dimensional gas chromatography (GCxGC) coupled with time-of-flight mass spectrometric (TOFMS) method was optimized for simultaneous analysis of 160 pesticides, 12 dioxin-like polychlorinated biphenyls (PCBs), 12 polyaromatic hydrocarbons (PAHs) and bisphenol A in grape and wine. GCxGC-TOFMS could separate all the 185 analytes within 38min with >85% NIST library-based mass spectral confirmations. The matrix effect quantified as the ratio of the slope of matrix-matched to solvent calibrations was within 0.5-1.5 for most analytes. LOQ of most of the analytes was < or =10microg/L with nine exceptions having LOQs of 12.5-25microg/L. Recoveries ranged between 70 and 120% with <20% expanded uncertainties for 151 and 148 compounds in grape and wine, respectively, with intra-laboratory Horwitz ratio <0.2 for all analytes. The method was evaluated in the incurred grape samples where residues of cypermethrin, permethrin, chlorpyriphos, metalaxyl and etophenprox were detected at below MRL.
authors.affiliation: National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India.
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Sangram H
authors.initials: SH
authors.lastname: Patil
authors.forename: Manoj
authors.initials: M
authors.lastname: Ghaste
authors.forename: K N
authors.initials: KN
authors.lastname: Dhumal
authors.forename: Pandurang G
authors.initials: PG
authors.lastname: Adsule
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D011078:Polychlorinated Biphenyls; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014508:Urea / Q000737:chemistry; D027843:Vitis / Q000737:chemistry*; D014920:Wine / Q000032:analysis*
chemical_list: D010573:Pesticide Residues; D014508:Urea; D011078:Polychlorinated Biphenyls