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

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. 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. 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%). 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. 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.