GERSTEL K.K., 1-3-1 Nakane, Tokyo 152-0031, Japan.
J Chromatogr A. 2012 Dec 28;1270:296-304. doi: 10.1016/j.chroma.2012.11.002. Epub 2012 Nov 8.
A method is described for characterization of sulfur compounds in unaged and aged whisky. The method is based on full evaporation dynamic headspace (FEDHS) of 100 μL of whisky samples followed by selectable one-dimensional ((1)D) or two-dimensional ((2)D) retention-time-locked (RTL) gas chromatography (GC)-mass spectrometry (MS) with simultaneous element-specific detection using a sulfur chemiluminescence detector (SCD) and a nitrogen chemiluminescence detector (NCD). Sequential heart-cuts of the 16 sulfur fractions were used to identify each individual sulfur compound in the unaged whisky. Twenty sulfur compounds were positively identified by a MS library search, linear retention indices (LRI), and formula identification using MS calibration software. Additionally eight formulas were also identified for unknown sulfur compounds. Simultaneous heart-cuts of the 16 sulfur fractions were used to produce the (2)D RTL GC-SCD chromatograms for principal component analysis. PCA of the (2)D RTL GC-SCD data clearly demonstrated the difference between unaged and aged whisky, as well as two different whisky samples. Fourteen sulfur compounds could be characterized as key sulfur compounds responsible for the changes in the aging step and/or the difference between two kinds of whisky samples. The determined values of the key sulfur compounds were in the range of 0.3-210 ng mL(-1) (RSD: 0.37-12%, n=3).
介绍了一种用于鉴定未陈酿和陈酿威士忌中含硫化合物的方法。该方法基于 100 μL 威士忌样品的全蒸发动态顶空（FEDHS），随后采用选择性一维（1D）或二维（2D）保留时间锁定（RTL）气相色谱（GC）-质谱（MS），同时使用硫化学发光检测器（SCD）和氮化学发光检测器（NCD）进行元素特异性检测。对 16 个硫馏分的顺序心切割用于鉴定未陈酿威士忌中的每个单独的含硫化合物。通过 MS 库搜索、线性保留指数（LRI）和使用 MS 校准软件进行公式鉴定，对 20 种含硫化合物进行了阳性鉴定。此外，还鉴定了 8 种未知含硫化合物的公式。对 16 个硫馏分的顺序心切割用于产生（2）D RTL GC-SCD 色谱图进行主成分分析。（2）D RTL GC-SCD 数据的 PCA 清楚地表明了未陈酿和陈酿威士忌以及两种不同威士忌样品之间的差异。可以将 14 种含硫化合物鉴定为负责老化步骤变化和/或两种威士忌样品之间差异的关键含硫化合物。关键含硫化合物的测定值在 0.3-210 ng mL（-1）（RSD：0.37-12%，n=3）范围内。
