Liquor vinasse is of interest under the biorefinery context and the aim of the present study was the recovery of flavour compounds. Supercritical carbon dioxide (SC‐CO 2 ) extraction is an optimal method for liquor vinasse flavour compounds recovery. Gas chromatography with mass spectrometry analysis showed that more than 50 compounds were identified in the SC‐CO 2 extract. The predominant compounds were esters and acids, and ethyl (9Z)‐9‐octadecenoate was the major ester. The effects of different extraction parameters, including pressure (8.2–41.8 MPa), temperature (32.8–67.2 °C) and CO 2 rate (6.4–23.6 l/h), on the yield of volatile compounds with SC‐CO 2 extraction were furthermore investigated. The most efficient extraction parameters for the maximum flavour compounds yield and better selection for ethyl (9Z)‐9‐octadecenoate were the following: pressure of 24.98 MPa, temperature of 51.28 °C and a CO 2 rate of 13.48 l/h.
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