白酒难挥发组分对白酒的风味品质具有重要的影响。采用滋味稀释分析技术(taste dilution analysis,TDA)结合仪器分析了酱香型白酒难挥发组分中的呈味化合物。以TDA感官强度为导向,结合固相萃取和多级高效液相色谱分离,从酱香型白酒难挥发组分中筛选并分离出3个关键呈味组分。进一步采用高分辨质谱和核磁共振技术解析了这些组分的化学结构,首次在白酒中鉴定出具有苦味特征的化合物9,10,13-三羟基-11(E)-十八烯酸(1)和9,12,13-三羟基-10(E)-十八烯酸(2)。基于超高效液相色谱串联三重四极杆技术建立了这2种三羟基十八烯酸在白酒中的精确定量方法。分析了它们在不同香型白酒样品中的含量,发现化合物1和2在酱香、浓香和清香型酒样中(共6种)均存在,质量浓度范围分别为1.8~265.3和2.2~111.3 μg/L,并且它们在酱香型酒样中浓度显著高于其他2种香型(p<0.01)。
The non-volatile component of Baijiu (Chinese liquor) has an important effect on overall flavor of the liquor. This study applied taste dilution analysis (TDA) to analyze the taste compounds in non-volatile component of Chinese Moutai-flavor type liquor. The experiment used human taste as a guide, combining with solid phase extraction and high performance liquid chromatography separation, to screen three taste-active fractions in non-volatile component of the liquor sample. These fractions were further analyzed by means of high resolution mass spectrometry and nuclear magnetic resonance. For the first time, bitter-tasting compounds 9,10,13-trihydroxyoctadec-11(E)-enoic acid (1) and 9,12,13-trihydroxyoctadec-10(E)-enoic acid (2) were identified in Chinese liquor. Based on ultra-high performance liquid chromatography-tandem mass spectrometry, a precise quantitative method for detection of the two trihydroxyoctadec acids in Chinese liquor was developed. The quantitative result revealed that compounds 1 and 2 were distributed in Chinese Moutai, strong and light-flavor type liquor samples (n=6), with range of 1.8-265.3 and 2.2-111.3 μg/L, respectively. Moreover, their concentrations in Moutai-flavor type liquor samples were significantly higher than those of other flavor types (p<0.01).
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