Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 24, Pages 3881-3889Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.04.003
Keywords
Grape; Wine; Pesticide residue; Comprehensive two-dimensional gas; chromatography time-of-Right mass; spectrometry; GC x GC-TOFMS; GC x GC optimization; Method validation; Measurement uncertainty; Dioxin-like polychlorinated biphenyls; Polyaromatic hydrocarbons
Funding
- APEDA, Government of India
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Two-dimensional gas chromatography (GC x 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 x 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 mu g/L with nine exceptions having LOQs of 12.5-25 mu g/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. (C) 2010 Elsevier B.V. All rights reserved.
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