Miniaturized QuEChERS method for determination of 97 pesticide residues in wine by ultra-high performance liquid chromatography coupled with tandem mass spectrometry

Abstract

A miniaturized sample preparation method was developed and validated for the multiresidue determination of 97 pesticides in wine samples. The proposed extraction procedure is based on the QuEChERS acetate method with dispersive solid phase extraction (d-SPE) for the clean-up step. Ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC-MS/MS) was used for determination. The extraction and clean-up steps were evaluated to obtain the best conditions for the selected pesticides. Miniaturization of the sample preparation step provided a reduction in the consumption of samples and chemicals. The method limit of quantification was between 10 and 20 μg L⁻¹. Trueness results, obtained by recovery assays at the spike levels 10, 20, 50 and 100 μg L⁻¹, ranged from 70 to 120% with precision in terms of relative standard deviations (RSD) ≤ 20%. The method was successfully applied for the analysis of wine samples and different pesticides were found at concentrations from 14 to 55 μg L⁻¹.