Combining headspace gas chromatography with mass spectrometry detection for confirmation of hydrocarbon residues in virgin olive oil following automatic screening

Hydrocarbon residues can be present in virgin olive oils either naturally or as contaminants. Presence of benzene, toluene, ethylbenzene, xylene isomers and styrene (BTEXS) in virgin olive oil, demanded the establishment of a cut-off level to discriminate oil samples containing these residues at normal levels from those at high levels caused by contamination. By introducing volatile components present in the headspace (HS) of the oil samples (without prior chromatographic separation) into the ionization source of a mass spectrometer, samples were classified as containing normal or high levels of BTEXS (recommendable or non-recommendable for human consumption). Confirmation and quantification of contaminated virgin olive oils were achieved by combining HS sampling with gas chromatography–mass spectrometry (GC–MS). No sample pretreatment was necessary for the chromatographic method, but the addition of 600 μl of ethyl acetate as chemical modifier for 10 ml of virgin olive oil. Detection limits ranged between 3 and 9 ng/ml. Oil analysis showed the presence of toluene in all samples, as well as the absence of benzene, ethylbenzene and o-xylene.