The use of headspace adsorbent traps in combination with gas chromatography was evaluated for the determination of volatile constituents (i.e. higher alcohols and other congeners of alcoholic fermentation) in spirits. The headspace trap technology comprises an enhanced static headspace system that allows enrichment and focusing of analytes on adsorbent traps prior to gas chromatographic separation. Extraction yields 35-55 times higher than those seen with static headspace sampling were achieved. An excellent agreement of analysis results in comparison to the European reference procedure was found (R > 0.98, p < 0.0001). The fully automated headspace trap procedure requires only minimal sample preparation and is easy to apply.