Gas chromatographic-mass spectrometric analysis of acids and phenols in distilled alcohol beverages - Application of anion-exchange disk extraction combined with in-vial elution and silylation

A GC-MS protocol for profiling spirits, based on 19 acids and phenolic comp ounds, has been proposed and evaluated. The method combined a simple precon centration procedure based on solid-phase (anion-exchange) disk extraction, and in-vial elution and silylation of the analytes. The derivatized extrac t was directly injected into the GC-MS system. These analytes were: C-6, C- 8, C-10, C-12 acids, pyruvic acid, 2-furoic acid, succinic acid, fumaric ac id, glutaric acid, lactic acid, glycolic acid, malic acid, tartaric acid, c itric acid, vanillin, syringaldehyde, coniferalldehyde, vanillic acid and g allic acid. The profiles of six different spirits were found reproducible f rom day-to-day with <20% RSD for measurements of most of the analytes at di fferent concentrations. Recoveries of individual analytes appear to be affe cted by the level of tannins in the spirits, and they varied from sample to sample. The method of standard addition was used to quantify age-related a nalytes. Good linearity of response with correlation coefficients in the ra nge of 0.992-0.999 was obtained. The results of the study indicate that for spirits of the same brand but of different ages, the amounts of these anal ytes appear to increase with the ageing period. (C) 2000 Elsevier Science B N. All rights reserved.