Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan.
General Research Laboratory, Kiku-Masamune Sake Brewing Co. Ltd., 1-8-6 Uozaki-nishimachi, Higashinada-ku, Kobe, Hyogo 658-0026, Japan.
J Biosci Bioeng. 2021 Jul;132(1):108-112. doi: 10.1016/j.jbiosc.2021.03.014. Epub 2021 May 1.
The combination of solid phase microextraction (SPME) and gas chromatograph-mass spectrometer (GC-MS) is frequently used for comprehensive analysis of aroma components in foods because it can be used to easily analyze volatile components, allowing saving of the amount of solvent used. In this study, SPME-GC-MS analysis of sake samples before and after sherry cask storage was performed to investigate the special flavor derived from sherry cask storage. A GC column with polyethylene glycol as the stationary phase, which is the first choice for volatile component analysis, was used. However, the peak of the acid having a carbonyl group was tailed due to its bond with the hydroxyl group of the stationary phase. In the analysis of sake samples, a large and tailing peak derived from the large amount of fatty acids in Japanese sake was observed. Additionally, it was not possible to analyze other co-eluting components. To overcome this problem, a novel extraction condition was examined using SPME and tris (hydroxymethyl) aminomethane (Tris). By adding Tris solution to sake, the fatty acid peak was removed successfully, thereby facilitating analysis of the peaks of compounds co-eluting with fatty acids and comprehensive analysis of the aroma components in sake. Furthermore, a comparative analysis of sake before and after storage in sherry cask showed that levels of fatty alcohols, organic acid esters, fatty acid esters, and terpenes increased significantly after storage in sherry cask, suggesting that these ingredients might constitute the special flavor of sherry cask-stored sake.
固相微萃取（SPME）和气相色谱-质谱联用（GC-MS）的组合常用于食品香气成分的综合分析，因为它可以轻松分析挥发性成分，节省溶剂用量。本研究采用聚乙二醇作为固定相的 GC 柱，这是挥发性成分分析的首选，对陈酿雪利桶前后的清酒样品进行了 SPME-GC-MS 分析，以研究来自雪利桶陈酿的特殊风味。然而，由于羰基与固定相的羟基结合，带羰基的酸的峰出现了拖尾。在清酒样品的分析中，观察到源自日本清酒中大量脂肪酸的大量拖尾峰。此外，无法分析其他共洗脱的成分。为了解决这个问题，使用 SPME 和三羟甲基氨基甲烷（Tris）检查了一种新的提取条件。通过向清酒中添加 Tris 溶液，成功去除了脂肪酸峰，从而便于分析与脂肪酸共洗脱的化合物的峰，并对清酒中的香气成分进行综合分析。此外，对陈酿前和陈酿后的清酒进行比较分析表明，陈酿后雪利桶中的脂肪醇、有机酸酯、脂肪酸酯和萜烯的水平显著增加，表明这些成分可能构成雪利桶陈酿清酒的特殊风味。
