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Abstract
A method based on a QuEChERS (quick, easy, cheap, effective, rugged, safe) sample preparation method and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) was developed for simultaneous determination of 77 pesticide residues in wine. An extraction of 10 ml of sample with acetonitrile followed by liquid–liquid partition formed by the addition of 4 g MgSO4 and 3 g NaCl was applied in the sample preparation. The clean-up was carried out by applying dispersive solid-phase with 150 mg MgSO4 as well as 50 mg primary secondary amine (PSA). One quantitation ion and at least two identification ions were selected in the analytical method for each pesticide compound by GC/MS. The recovery data were obtained by spiking blank samples at two concentration levels (0.05 and 0.2 mg l−1). The recoveries of all pesticides were in the range 70–110%, with intra-day precision of less than 15%, and the inter-day precision of less than 22% and 15% for 0.05 and 0.2 mg l−1 fortification levels, respectively. Linearity was between 0.02 and 2 mg l−1 with determination coefficients (R 2) greater than 0.98 for all compounds. The limits of quantification (LOQs) for the 77 pesticides ranged from 0.003 to 0.05 mg l−1. This method was applied for routine analysis in market products.
Acknowledgements
This study was supported by a Fund from the Ministry of Heath, China (Project Number WKJ2006-2-10) China Postdoctoral Foundation (No. 20080440456) and partially supported by an ‘863’ Project from the Ministry of Science, China (Project Number 2007AA10Z433).
