Ng L K, Lafontaine P, Harnois J
Laboratory and Scientific Services Directorate, Canada Customs and Revenue Agency, Ottawa, Ontario, Canada.
J Chromatogr A. 2000 Mar 17;873(1):29-38. doi: 10.1016/s0021-9673(99)01100-0.
A GC-MS protocol for profiling spirits, based on 19 acids and phenolic compounds, has been proposed and evaluated. The method combined a simple preconcentration procedure based on solid-phase (anion-exchange) disk extraction, and in-vial elution and silylation of the analytes. The derivatized extract was directly injected into the GC-MS system. These analytes were: C6, C8, C10, C12 acids, pyruvic acid, 2-furoic acid, succinic acid, fumaric acid, glutaric acid, lactic acid, glycolic acid, malic acid, tartaric acid, citric acid, vanillin, syringaldehyde, coniferaldehyde, vanillic acid and gallic acid. The profiles of six different spirits were found reproducible from day-to-day with <20% RSD for measurements of most of the analytes at different concentrations. Recoveries of individual analytes appear to be affected 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 analytes. Good linearity of response with correlation coefficients in the range 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 analytes appear to increase with the ageing period.
一种基于19种酸和酚类化合物的用于烈酒成分分析的气相色谱 - 质谱联用（GC-MS）方法已被提出并评估。该方法结合了基于固相（阴离子交换）圆盘萃取的简单预浓缩程序，以及分析物的瓶内洗脱和硅烷化处理。衍生化提取物直接注入GC-MS系统。这些分析物包括：己酸、辛酸、癸酸、月桂酸、丙酮酸、糠酸、琥珀酸、富马酸、戊二酸、乳酸、乙醇酸、苹果酸、酒石酸、柠檬酸、香草醛、丁香醛、松柏醛、香草酸和没食子酸。六种不同烈酒的成分分析结果在不同日期具有可重复性，对于不同浓度的大多数分析物，相对标准偏差（RSD）<20%。单个分析物的回收率似乎受烈酒中单宁含量水平的影响，并且因样品而异。采用标准加入法对与年份相关的分析物进行定量。获得了良好的线性响应，相关系数范围为0.992 - 0.999。研究结果表明，对于同一品牌但不同年份的烈酒，这些分析物的含量似乎随着陈酿时间的增加而增加。
