Determination of 103 Pesticides and Their Main Metabolites in Animal Origin Food by QuEChERS and Liquid Chromatography–Tandem Mass Spectrometry

Abstract

A rapid and sensitive analytical multiresidue method has been developed for the simultaneous determination of 103 pesticides (herbicides, insecticides, and fungicides) and 18 metabolites in foods of animal origin using liquid chromatography-tandem with triple quadrupole in dynamic multiple reaction monitoring (DMRM) mode. A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation technique was established, and the efficiency of the dispersive solid-phase extraction (d-SPE) cleanup step was evaluated by comparing the effects of different d-SPE sorbent combinations (primary secondary amine (PSA) + graphitized carbon black (GCB), PSA + C18, C18, and C18 + GCB). The limits of quantification (LOQs) ranged from 1 to 10 μg/kg, and the coefficient of determination (R 2) was ≥0.995 within the calibration linearity range of 0–250 μg/L for all pesticides. The combination of C18 + GCB was validated at two spiking levels (10 and 50 μg/kg) in chicken, fish, pork, and rabbit. Satisfactory recoveries (70–119%) and RSDs ≤17% were achieved for all analytes, except for naptalam (60–69%), pyrimethanil (40–49%), and thiabendazole (62–66%) at 10 μg/kg spiking level. The validated method was successfully applied to the analysis of real samples of food of animal origin.