A multi-residue pesticide determination in fatty food commodities by modified QuEChERS approach and gas chromatography-tandem mass spectrometry

A QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) based multi-residue method has been developed and validated for the extraction and determination of pesticides in fatty matrices by gas chromatography tandem mass spectrometry. Extraction and clean-up were performed according to QuEChERS principles widely used for non-fatty matrices, with main difference, a higher solvent/sample- ratio followed by a 6-fold preconcentration step, ensuring good extractability and sensitivity. A validation according to SANTE guidelines was performed using a olive and sunflower oils mixture 1:1, w/w as representative matrix, at 2 concentration levels (5 and 50 µg/kg) targeting 176 GC-amenable pesticides. Most compounds fulfilled the validation criteria, with a limit of quantification of 5 µg/kg for 137 compounds , and of 50 µg/kg for 24 compounds. Afterwards, the method performance was tested in six different fatty matrices with 73–90% of the analytes fulfilling the performance criteria at 5 µg/kg depending on the matrix.