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A method for the multiresidue determination of 35 pesticides (30 insecticides and five herbicides) in olive oil by gas chromatography (GC) is described. Three liquid-liquid extraction (LLE) procedures based on (i) partition of pesticides between acetonitrile (ACN) and oil solution in n-hexane, (ii) partition of pesticides between saturated ACN with n-hexane and oil solution in n-hexane saturated with ACN, and (iii) partition of pesticides between ACN and oil were tested for the optimization of the highest pesticide recoveries with the lowest oil residue in the final extracts. Experimental tests were preformed in order to study the efficiency of different clean up procedures with N-Alumina, Florisil, C18, and ENVI-Carb solid-phase extraction (SPE) cartridges for the compounds analyzed by GC-nitrogen phosphorus detection. A second step of clean up was also performed for the compounds analyzed by GC-electron capture detection (ECD), by using phenyl-bonded silica (Ph), diol-bonded silica (Diol), cyanopropyl-bonded silica (CN), and amino propyl-bonded silica (NH2) SPE cartridges. LLE of the oil solution in hexane with ACN followed by an ENVI-Carb SPE clean up of the extract gave the best results for all target compounds. The ACN extract was additionally cleaned through a Diol-SPE cartridge for the determination of pesticides analyzed mainly by GC-ECD. Pesticide recoveries form virgin olive oil spiked with 20, 100, and 500 microg/kg concentrations of pesticides ranged from 70.9 to 107.4%. The proposed method featured good sensitivity, pesticide quantification limits were low enough, and the precision, expressed as relative standard deviation, ranged from 2.4 to 12.0%. The proposed method was applied successfully for the residue determination of the selected pesticides in commercial olive oil samples.

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The processing factors (pesticide concentration found in olive oil/pesticide concentration found in olives) of azinphos methyl, chlorpyrifos, lambda-cyhalothrin, deltamethrin, diazinon, dimethoate, endosulfan, and fenthion were determined in olive oil production process in various laboratory-scale olive oil extractions based on three- or two-phase centrifugation systems in comparison with samples collected during olive oil extractions in conventional olive mills located at different olive oil production areas in Greece. Pesticide analyses were performed using a multiresidue method developed in our laboratory for the determination of different insecticides and herbicides in olive oil by solid-phase extraction techniques coupled to gas chromatography detection (electron capture detection and nitrogen phosphorus detection), optimized, and validated for olive fruits sample preparation. Processing factors were found to vary among the different pesticides studied. Water addition in the oil extraction procedure (as in a three-phase centrifugation system) was found to decrease the processing factors of dimethoate, alpha-endosulfan, diazinon, and chlorpyrifos, whereas those of fenthion, azinphos methyl, beta-endosulfan, lambda-cyhalothrin, and deltamethrin residues were not affected. The water content of olives processed was found to proportionally affect pesticide processing factors. Fenthion sulfoxide and endosulfan sulfate were the major metabolites of fenthion and endosulfan, respectively, that were detected in laboratory-produced olive oils, but only the concentration of fenthion sulfoxide was found to increase with the increase of water addition in the olive oil extraction process.

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