Pesticide residues analysis in wine by liquid chromatography–tandem mass spectrometry and using ethyl acetate extraction method: validation and pilot survey in real samples

Abstract

This paper presents a cost-effective and validated method for the determination of 172 pesticide residues monitored during a survey study on 27 commercially available Cypriot wines (red/white, dry/sweet). Sample preparation involved ethyl acetate extraction of pesticides from wines. For the validation of the method, blank samples were spiked with a solution of 172 pesticides (such as insecticides, fungicides, herbicides) at three levels such as 0.01, 0.05 and 0.1 mg/kg. The samples were analyzed by LC-MS/MS (liquid chromatography tandem mass spectrometry). The validation study was in accordance with the DG SANCO (Directorate-General for Health and Consumers) guidelines [Document No. SANCO/12495/2012. Method validation and quality control procedures for pesticide residues analysis in food and feed]. The scope of validation included recovery, linearity, limits of quantification and precision. Recoveries of the majority of compounds were found to be in the range of 70–120% and were characterized by precision lower than 20%. Fifteen out of the 27 real samples analyzed were positive with pesticide residues and all observed values were much lower than the MRLs.