Department of Chemical, Biological, Pharmaceutical and Environmental Sciences, University of Messina, Messina, Italy; Institute of Chemical Technology and Analytics, Vienna University of Technology, Getreidemarkt 9/164, Vienna 1060, Austria.
Institute of Chemical Technology and Analytics, Vienna University of Technology, Getreidemarkt 9/164, Vienna 1060, Austria; Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki 54124, Greece.
J Chromatogr A. 2022 Aug 2;1676:463241. doi: 10.1016/j.chroma.2022.463241. Epub 2022 Jun 15.
We present a novel sample preparation method for the extraction and preconcentration of volatile organic compounds from whiskey samples prior to their determination by comprehensive two-dimensional gas chromatography (GC × GC) coupled to mass spectrometry (MS). Sample preparation of the volatile compounds, important for the organoleptic characteristics of different whiskeys and their acceptance and liking by the consumers, is based on the use of the solid-phase microextraction (SPME) Arrow. After optimization, the proposed method was compared with conventional SPME regarding the analysis of different types of whiskey (i.e., Irish whiskey, single malt Scotch whiskey and blended Scotch whiskey) and was shown to exhibit an up to a factor of six higher sensitivity and better repeatability by a factor of up to five, depending on the compound class. A total of 167 volatile organic compounds, including terpenes, alcohols, esters, carboxylic acids, ketones, were tentatively-identified using the SPME Arrow technique, while a significantly lower number of compounds (126) were determined by means of conventional SPME. SPME Arrow combined with GC × GC-MS was demonstrated to be a powerful analytical tool for the exploration of the volatile profile of complex samples, allowing to identify differences in important flavour compounds for the three different types of whiskey investigated.
我们提出了一种新颖的样品制备方法，用于在通过二维气相色谱（GC×GC）与质谱（MS）联用对威士忌样品中的挥发性有机化合物进行测定之前，从威士忌样品中提取和预浓缩挥发性有机化合物。对于不同威士忌的感官特性及其被消费者接受和喜爱的重要挥发性化合物的样品制备，基于固相微萃取（SPME）Arrow 的使用。在优化后，将所提出的方法与常规 SPME 进行了比较，分析了不同类型的威士忌（即爱尔兰威士忌、单一麦芽苏格兰威士忌和混合苏格兰威士忌），结果表明，根据化合物的类别，该方法的灵敏度提高了高达六倍，重复性提高了高达五倍。使用 SPME Arrow 技术，共鉴定出 167 种挥发性有机化合物，包括萜烯、醇、酯、羧酸、酮，而通过常规 SPME 仅确定了数量明显较少的化合物（126 种）。SPME Arrow 与 GC×GC-MS 相结合被证明是一种强大的分析工具，可用于探索复杂样品的挥发性特征，能够鉴定出所研究的三种不同类型威士忌中重要风味化合物的差异。
