High-throughput multi-residue determination of 157 pesticides in wine using QuEChERS-UPLC-MS/MS for routine...

A rapid and reliable multi-residue analytical method was developed for the simultaneous determination of 157 pesticide residues in wine using QuEChERS extraction followed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The extraction protocol included two extract-treatment pathways to enable the determination of acidic pesticides as well as compounds with different stability under acidic or basic conditions. The method was validated according to the SANTE guidelines for pesticide residue analysis. Matrix-matched calibration curves showed good linearity for all analytes, with correlation coefficients (R²) ranging from 0.9866 to 0.9994 within the concentration range of 0.005-0.080 mg kg^-1 and the limits of detection (LOD) and quantification (LOQ) were established at 0.0033 mg kg^-1and 0.010 mg kg^-1, respectively. Recovery values ranged from 72 to 116%, while repeatability (RSD_r) and within-laboratory reproducibility (RSD_R) were ≤15.2% and ≤19.7%, respectively. Expanded measurement uncertainty ranged from 5 to 42% (k = 2). The validated method was applied to commercial wine samples, where several pesticide residues were detected at concentrations between 0.0082 and 0.1881 mg kg^-1. The developed method demonstrated high suitability for high-throughput routine monitoring and large-scale surveillance of pesticide residues in wine due to its sensitivity, accuracy and rapid analysis time.