Modification and validation of the simultaneous detection of 38 pesticide residues method by ultra‐high‐performance liquid chromatography/tandem mass spectrometry with QuEChERS extraction in different oil crops and products

Abstract

Oil crops and products are important food materials in daily life. Pesticide residues in food could directly and indirectly endanger human health. However, the method for detecting multiple pesticides simultaneously is limited. In this study, an easy and efficient method for the simultaneous determination of 38 pesticides in oil crops and products was established and validated. All samples were treated with a modified QuEChERS procedure followed by ultra-high-performance liquid chromatography/tandem mass spectrometry (UHPLC/MS/MS) analysis. Mass spectrometry was performed in positive and negative ion electrospray ionization mode. The mobile phase consisted of 0.1% formic acid in water and 0.1% formic acid in acetonitrile. The column used was a Poroshell 120 EC-C18 and the flow rate was 0.3 mL/min. The method was validated so that the calibration curves for all pesticides had good linearity in the concentration range of 10-1000 μg/L with correlation coefficients (R2 ) above 0.9945. The recovery rates were between 70.1 and 120.0%, with relative standard deviations (RSDs) (n = 6) ≤20.0%. The limits of quantification (LOQs) ranged from 0.5 to 10 μg/kg, limits of detection (LODs) ranged from 2.0 to 30 μg/kg, and the matrix effect (ME) ranged from -18.77 to 19.33%, respectively. The method proved to be accurate, sensitive, and stable. It can be used for rapid screening and confirmation of 38 pesticide residues in oil crops and products which takes 10 min for sample extraction and clean-up with less requirement of solvents. This study provides a technical basis for regulatory analysis and quality supervision of foods.