The use of a new technique combining low-temperature vacuum distillation with a specific chemical capture with an organomercuric compound enabled the extraction of volatile odorous thiols present at very low concentrations in the Bordeaux red wine varieties Merlot and Cabernet Sauvignon. The analysis of wine extracts by gas chromatography coupled with detection by olfactometry, flame photometry, and mass spectrometry led to the identification of three aromatic thiols: 3-mercapto-2-methylpropanol, identified for the first time in wine; 3-mercaptohexanol; and 3-mercaptohexyl acetate, already described in Sauvignon Blanc wines.