Development of a Rapid Method for Simultaneous Determination of Pesticides in Plant Oil Using GC-MS/MS

Multi-residue methodologies necessitate a tailored and precise approach across all areas of analysis. Analyte extraction must be closely correlated with the sample matrix to ensure the optimal recovery for the maximal array of analytes, thereby fulfilling all legal requirements concerning analytical determination. Although the QuEChERS method offers undeniable advantages, it proves unsuitable for pesticide residue determination in matrices with high oil contents. A pivotal component of the method involves employing n-hexane as the extraction solvent and utilizing solvent exchange in obtaining the final extract. The analytical method developed by our laboratory, as presented here, enabled the determination of all requisite pesticides in accordance with European Union (EU) Regulation 396/2005. The linearity, limits of detection and quantification, matrix effects, accuracy, and precision of the method were evaluated in line with the aforementioned regulation. Of the analyzed pesticide residues, 273 exhibited expanded uncertainty with an RSDr ≤ 20%, with recoveries falling within the range of 70–120%, meeting all the requirements of document SANTE/11312/2021 V2. For 9 pesticides, the recovery was below 30%, and the precision of the obtained content for 21 compounds surpassed 20%, necessitating the removal of these compounds from the analytical method.