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A Quick and Inexpensive Method to Determine Pesticide Residues in Olive Oil by UHPLC-MS/MS and GC-MS/MS

Olive oil samples were analyzed for twenty-nine pesticides by means of gas chromatography and Ultra HPLC coupled to mass spectrometry. The list of the investigated pesticide residues includes the twenty-seven pesticide residues of the target protocol of COIPT proficiency tests, yearly organized in our laboratory. The sample preparation procedure was based on acetonitrile extraction and on line cleanup C18 cartridges. The method was rapid, inexpensive and with a sufficient cleanup to reduce the effect of a complex matrix such as the olive oil. The method was validated according to EU guidelines, including the estimation of the uncertainty measurement. In the estimation also the recovery component was considered, when a correction factor was applied during the calculation. The dispersion of the individual recovery results (obtained collecting both the ongoing validation and QC data from the routine analysis) did not show a positive or negative bias but rather a symmetry of the data highlighting a normal distribution. So it was possible to support also a good robustness of the method, in particular the overall mean recovery was a value of 99% and the within-laboratory reproducibility (RSDWR), derived from on-going method validation and routine quality control, was a value of 13%.