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 |
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Authors: | Soma Dasgupta Kaushik Banerjee Sangram H Patil Manoj Ghaste KN Dhumal Pandurang G Adsule |
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Institution: | 1. National Research Centre for Grapes, P.O. Manjri Farm, Pune 412 307, India;2. Department of Environmental Sciences, University of Pune, Pune 411 007, India;3. Department of Botany, University of Pune, Pune 411 007, India |
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Abstract: | 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 38 min 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 ≤10 μg/L with nine exceptions having LOQs of 12.5–25 μg/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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Keywords: | Grape Wine Pesticide residue Comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry GC × GC&ndash TOFMS GC × GC optimization Method validation Measurement uncertainty Dioxin-like polychlorinated biphenyls Polyaromatic hydrocarbons |
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