Multiresidue method for the determination of 77 pesticides in wine using QuEChERS sample preparation and gas chromatography with mass spectrometry

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.

Keywords:

• multiresidue
• QuEChERS (quick; easy; cheap; effective; rugged; safe)
• gas chromatography-mass spectrometry by selected ion monitoring (GC/MS-SIM)
• wine
• pesticide; analysis

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).