Abstract
Distilled spirits can be very complex in their sensory or organoleptic compounds. Of significant interest is determination of the concentration of methanol, ethyl acetate, and fusel oils, which include n-propanol, isobutanol, n-butanol, active amyl (2-methyl-1-butanol) and isoamyl (3-methyl-1-butanol) alcohols. Here, we describe a validated method for the analysis of these analytes using a headspace (HS) sampling unit coupled with a gas chromatograph fitted with a flame ionization detector (GC/FID) for profiling these analytes in distilled spirits (n = 26) obtained from local retailers. HS results were compared to the direct injection (DI) GC/FID protocol made available by the US Alcohol and Tobacco Tax and Trade Bureau (TTB), method SSD:TM:200 via correlation and Bland-Altman difference plots to demonstrate that HS-GC/FID is a valid alternative to the direct injection protocols described elsewhere. •A method for the analysis of methanol, ethyl acetate, and fusel oils via headspace sampling coupled to a gas chromatograph fitted with a flame ionization detector (HS-GC/FID) is described.•Samples required no pre-treatment beyond diluting 1 mL of distilled spirit in 4 mL water containing table salt, which resulted in a method with minimal inlet or column maintenance, little sample prepration, and a rapid run time with retention times under 7 min.•Validation by comparing to established protocols using direct injection made available by the US Federal Tax and Trade Bureau (TTB).