Analytical Characterization of the Flavor of Oxygen-Spoiled Wines through the Gas Chromatography--Ion-Trap Mass Spectrometry of Ultratrace Odorants: Optimization of Conditions

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Abstract
A method for the direct determination of the most important aromas generated in oxygen-spoiled wines is developed. The method allows the simultaneous determination of some key ultratrace carbonyls, such as t-2-hexenal, t-2-octenal, and t-2-nonenal; other carbonyls such as furfural, 5-methyl furfural, hexanal, and benzaldehyde; some alcohols, such as 1 -octen-3-ol, 2-buthoxyethanol, and furfurol; and a volatile phenol, such as eugenol. Only one internal standard is used, and chemical derivatization of carbonyls is not required. The method combines a powerful preconcentration based on the demixture of an alcoholic fraction by salting out the wine with a liquid—liquid microextraction of an ether—pentane (10:90) mixture. The first step guarantees sensitivity, and the second step ensures selectivity and cleanliness. The extract, which is enriched between 200- and 2000-fold in the analytes, is directly injected into the gas chromatography—ion-trap mass spectrometry system. The preconcentration, injection, and mass-selective detection analysis steps have been optimized with both synthetic and real extracts in order to reach a reasonable compromise among sensitivity, selectivity, and cleanliness. The method is free from matrix effects, and linearity is satisfactory. The global method reproducibility ranges from 3 to 7% for most of the analytes. Detection limits range from 10 to 600 ng/L.

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