Determination of Pesticides and PCBs in Virgin Olive Oil by Multicolumn Solid-Phase Extraction Cleanup Followed by GC-NPD/ECD and Confirmation by Ion-Trap GC−MS

A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C18) and normal (alumina) phase SPE columns. Determination of OPs was by GC-NPD, while the OCs and PCBs were analyzed using GC-ECD. Recovery assays for OPs varied from 81.7% to 105.3%, for OCs ranged between 74.3% and 99.4%, while for PCBs were from 60.1% to 119.2%. Quantitation limits ranged from 10 to 25 μg/kg olive oil for OPs, and from 1 to 6 μg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC−MS/MS. The applicability of the method was assayed with 19 virgin olive oil samples collected from different olive mills of Aragón (Spain). Only one OP pesticide (acephate) was detected in one sample at a concentration of 10 μg/kg. Organochlorine pesticides were found in 5−47% of samples at very low levels ranging from 1.5 to 5.2 μg/kg. PCBs were found in 20−90% of samples, showing concentrations between 2.3 and 17.3 μg/kg. Keywords: Virgin olive oil; organophosphorus pesticides; organochlorine pesticides; polychlorinated biphenyls; capillary gas chromatography−mass spectrometric detection