Suitability of microwave-assisted extraction coupled with solid-phase extraction for organophosphorus pesticide determination in olive oil

A systematic study of the microwave-assisted extraction coupled to solid-phase extraction of nine organophosphorus pesticides (dimethoate, diazinon, pirimiphos methyl, parathion methyl, malathion, fenthion, chlorpyriphos, methidathion and azinphos methyl) from olive oil is described. The method is based on microwave-assisted liquid–liquid extraction with partition of organophosphorus pesticides between an acetonitrile–dichloromethane mixture and oil. Cleanup of extracts was performed with ENVI-Carb solid-phase extraction cartridge using dichloromethane as the elution solvent. The determination of pesticides in the final extracts was carried out by gas chromatography–flame photometric detection and gas chromatography–tandem mass spectrometry, using a triple quadrupole mass analyzer, for confirmative purposes. The study and optimization of the method was achieved through experimental design where recovery of compounds using acetonitrile for partition ranged from 62 to 99%. By adding dichloromethane to the extracting solution, the recoveries of more hydrophobic compounds were significantly increased. Under optimized conditions recoveries of pesticides from oil were equal to or higher than 73%, except for fenthion and chlorpyriphos at concentrations higher than 0.06 μg g−1 and diazinon at 0.03 μg g−1, with RSDs equal to or lower than 11% and quantification limits ranging from 0.007 to 0.020 μg g−1. The proposed method was applied to residue determination of the selected pesticides in commercial olive and avocado oil produced in Chile.