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

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726.233~1 290.769 mg/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-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。

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

34 flavor compounds,including 8 alcohols,14 esters,4 aldehydes,5 acids,1 phenol,1 lactone,and 1 heterocycle,were determined in rice wine by solid-phase micro extraction and gas chromatograph-mass spectrometer.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 μg/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 β-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 aging increased because of the esterification and transesterification reaction.In addition,aldehydes during aging also increased 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.