Determination of important odor-active aldehydes of wine through gas chromatography-mass spectrometry of their O-(2,3,4,5,6-pentafluorobenzyl)oximes formed directly in the solid phase extraction cartridge used for selective isolation

A method for the quantitative determination of octanal, nonanal, decanal, (E)-2-nonenal and (E, Z)-2,6-nonadienal in wine has been developed. In the proposed method, 200 ml of wine percolate through a solid phase extraction (SPE) cartridge packed with 200 mg of LiChrolut EN resins. The interferences are eluted with 60 ml of an aqueous solution containing 40% of methanol and 1% of NaHCO3. In the same SPE cartridge, the corresponding O-(2,3,4,5,6-pentafluorobenzyl)oximes are formed by letting percolate 2 ml of the reagent solution (5 mg ml(-1)). At room temperature the derivatization goes to completion in 15 min. The derivatives are eluted with 2 ml of dichloromethane, and the extract is concentrated and then analyzed by gas chromatography-mass spectrometry (GC-MS). The percentage of recovery in the isolation process is better than 90% in all cases with the exception of octanal, and is independent of the wine studied. In the cases of octanal, nonanal and decanal, the detection limits of the method are determined by the contamination levels of the reagent itself, and vary between 160 and 380 ng l(-1). For (E)-2-nonenal and (E, Z)-2,6-nonadienal, the detection limits were 12 and 20 and ng l(-1), respectively. The linearity of the method upheld until 10 mug l(-1) and was satisfactory in all cases. The reproducibility of the method is independent of the concentration and ranges from 30 to 190 ng I`. The method has been applied to the analysis of these components in several wine samples. With the exception of (E, Z)-2,6-nonadienal, all the components can reach concentrations above their corresponding odor threshold values. (C) 2004 Elsevier B.V. All rights reserved.