Multiclass Multipesticide Residue Analysis in Fish Matrix by a Modified QuEChERS Method Using Gas Chromatography with Mass Spectrometric Determination

Background: Pesticide residue in fish is a global food safety concern. However, very few validated methods are available targeting simultaneous analysis of multiple classes of pesticides. Objective: The aim of this study was to validate a quick, easy, cheap, effective, rugged, and safe workflow–based method for the quantitative determination of multiclass pesticides in fish matrix using GC-MS determination. Method: The sample was extracted with acetonitrile, and the cleanup method involved dispersive solid-phase extraction with C-18 sorbent, which effectively scavenged the coextracted matrix components and removed those from the extract. The data on recovery and precision of the method satisfied the criteria of SANTE/11813/2017 guidelines. Average recoveries of pesticides were in the range of 80–120% with precision RSDs ≤20%. The LOD and LOQ were in the ranges of 0.001–0.029 and 0.005–0.125 µg/mL, respectively, for all pesticides. The expanded uncertainty was in the range of 14–20%, based on the single-laboratory validation data (coverage factor, k = 2, confidence level, 95%). Conclusions: The validation data prove that the method is convenient and acceptable for the routine analysis of multiclass pesticide residues in fish matrices for regulatory compliance. Highlights: The study achieves multiresidue analysis of pesticides in fish matrix with MS-based confirmation. The method combines the advantages of nontarget analysis based on National Institute of Standards and Technology library matching in full scan mode with selected-ion monitoring–based sensitivity.