固相微萃取与气相色谱-质谱联用法对不同酒龄黄酒的微量风味分析与应用

Analysis and Application of Trace Compounds in Rice Wine by Solid-Phase Micro Etraction and Gas Chromatograph-Mass Spectrum

通过固相微萃取-气相色谱-质谱联用法检测了黄酒中34种风味成分，即醇类8种、酯类14种、醛类4种、酸类5种、酚类1种、内酯类1种和杂环类1种，该法精密度为4．42％～13．44％，回收率为78．44％～118．92％，检出限为0．002—13．92μg／L，该法准确可靠、操作简便。利用该法检测了不同酒龄的黄酒，发现黄酒中所测的风味化合物含量总和为726．233～1290．769mg／L-1，醇类、酯类和醛类是黄酒的主体香气，分别占风味化合物含量总和的63．68％-71．10％、27．84％～34．09％、〈2％。黄酒中主要化合物依次为β-苯乙醇、乳酸乙酯、异戊醇、异丁醇、乙酸乙酯、丁二酸二乙酯和2，3-丁二醇等。醇类在陈酿期间呈下降趋势，表明醇类主要是酿造过程产生，这是醇不断被氧化成酸所致；酯类是酒体变得醇香浓郁的重要原因，在陈酿期间呈先下降而后上升的趋势，这可能是陈酿后期醇酸酯化反应或酯交换的原因；醛类呈上升趋势，主要是陈酿过程中经高级醇的氧化或美拉德反应而来，其中5一甲基糠醛、糠醛和苯甲醛增加比例在10～40倍之间，是黄酒老化的重要指示剂。

34 flavor compounds, including 8 alcohols, 14 esters, 4 aldehydes, 5 acids, 1 phenol, 1 lactone, and 1 heteroeycle, were determined in rice wine by solid-phase micro extraction and gas chromatograph-mass spec- trometer. The precisions of the method ranged from 4.42% to 13.44%. The recoveries were 78.44% -118.92% with the detection limits in the range of 0. 002 - 13.92 txg/L. All data above-mentioned demonstrated it was a good method. Rice wine with different ages determined by this method. The total content of flavor compounds ranged from 726. 233 mg/L to 1290. 769 mg/L. The main compounds in rice wine were alcohols, esters and aldehydes, accounting for 63.68% - 71.10% , 27.84% - 34.09% , lower than 2% , respectively. Compounds with high content in rice wine in order were 13-phenylethanol, ethyl lactate, iso-pentyl alcohol, isobutanol, ethyl acetate, diethyl succinate, 2, 3-butanediol and so on. The alcohols during aging decreased due to the oxidation, while the esters during the later ag- ing increased because of the esterification and transesterification reaction. In addition, aldehydes during aging also in- creased by oxidation and maillard reaction. 5-methyl-2-furaldehyde, furfural and benzaldehyde increased by 10～40 times during aging demonstrated those three compounds could be used as aging indicators of rice wine.