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
2010
Dasgupta, Soma | Banerjee, Kaushik | Patil, Sangram H. | Ghaste, Manoj | Dhumal, K.N. | Adsule, P. G. (Pandurang G)
Two-dimensional gas chromatography (GC×GC) 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. GC×GC-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 ≤10μg/L with nine exceptions having LOQs of 12.5-25μg/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.
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