The extraction procedures (solid/liquid SPE and liquid/liquid LLE) and HPLC separation and quantification methods of polyphenolic compounds have been checked in virgin olive oils in order to explain the differences in content reported in the literature. The work has been carried out on oils prepared from one cultivar and produced under the same protocol. The extraction methods are practically equivalent, but the SPE technique is more favorable because it is faster and simpler. It has been proved that the chromatographic features and the method of chemical expression of the concentrations may greatly affect the final values. Thus, under the same analytical method, the total concentration values of polyphenols of the same oil show variations from 18% to 80%, according to the formality of expression as gallic acid, caffeic acid, or tyrosol equivalents. The role of the nature and spectrophotometric features of the phenols and of the internal standard is also discussed, and it was found to be an important source of reported variation. A gradient separation with an eluent mixture acetonitrile-sulfuric acid (0.1 mol/L), detection at 225 nm, and quantitative calculation of polyphenolic compounds in oils (expressed as tyrosol equivalents, THY(eq)) is proposed.

Volatile organic compounds strongly contribute to both the positive and negative sensory attributes of virgin olive oil, and more and more studies have been published in recent years focusing on several aspects regarding these molecules. This Review is aimed at giving an overview on the state of the art about the virgin olive oil volatile compounds. Particular emphasis was given to the composition of the volatile fraction, the analytical issues and approaches for analysis, the sensory characteristics and interaction with phenolic compounds, and the approaches for supporting the Panel Test in virgin olive oil classification and in authentication of the botanical and geographic origin based on volatile compounds. A pair of detailed tables with a total of approximately 700 volatiles identified or tentatively identified to date and tables dealing with analytical procedures, sensory characteristics of volatiles, and specific chemometric approaches for quality assessment are also provided.

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Evolution of the volatile profile of two extra-virgin olive oils with very different fatty acid composition (monounsaturated fatty acid/polyunsaturated fatty acid ratio) stored in several nonaccelerated oxidative conditions was studied by a validated headspace solid-phase microextraction-gas chromatography–mass spectrometry (HS-SPME-GC–MS) method. The role of C8 volatile compounds in oxidative processes was highlighted, and controversial aspects regarding the origin of some volatiles were clarified. Specific volatile markers for rancidity were proposed: sum of pentanal, hexanal, nonanal, E-2-heptenal, propanoic acid, and hexanoic acid for oils stored in the dark; sum of pentanal, heptanal, nonanal, decanal, E-2-heptenal, E-2-decenal, E,E-hepta-2,4-dienal, and E,E-deca-2,4-dienal, octane for oils stored under light exposure; sum of pentanal, nonanal, decanal, E-2-heptenal, E-2-decenal, E,E-hepta-2,4-dienal, nonan-1-ol, propanoic acid, octane, 6-methylhept-5-en-2-one, and oct-1-en-3-ol for oils stored under light exposure with oxygen in headspace. A simplified marker (sum of pentanal, nonanal and E-2-heptenal) suitable for all conditions was also proposed.