HS-SPME-GC-O-MS分析红枣发酵酒中的挥发性成分

Analysis of Volatile Compounds in Fermented Chinese Jujube Wine by Headspace Solid Phase Micro-Extraction and Gas Chromatography-Olfactometry-Mass Spectrometry

采用顶空固相微萃取、气相色谱-嗅闻-质谱(gas chromatography-olfactometry-mass spectrometry,GC-O-MS)联用,对红枣发酵酒中易挥发性成分进行萃取条件及GC-MS分离检测条件的系统研究,并采用气味活度值结合香气强度值评价了主要成分对总体香味的贡献。选定的顶空固相微萃取最优参数为:50/30μm DVB/CAR/PDMS固相微萃取头、样品用量8.0 m L/20.0 m L样品瓶、加盐量0.40 g/m L、萃取温度55℃、萃取时间40 min、平衡时间20 min、解吸时间5 min。选用Rtx-Wax色谱柱,经GC-O-MS联用对红枣发酵酒挥发性成分进行分析,共检出108种组分,结构推断86种,占挥发性成分总峰面积的97.09%。其中,乙酸-3-甲基丁酯、3-甲基丁醇、己酸乙酯、2-己烯酸乙酯、庚酸乙酯、乙酸、辛醇、癸酸乙酯、苯甲酸乙酯、戊酸、乙酸-2-苯乙酯、己酸、苯甲醇、苯丙酸乙酯、苯乙醇、辛酸、n-癸酸为红枣发酵酒的主体香气成分。其结果为红枣发酵酒的质控及香味评价提供一定理论依据。

The volatile compounds in fermented Chinese jujube wine were analyzed by headspace solid phase microextraction(HS-SPME)and gas chromatography-olfactometry-mass spectrometry(GC-O-MS).Extraction and GC-MSconditions were systematically studied and the contributions of the main components to the overall aroma of fermentedChinese jujube wine were evaluated by odor activity value(OAV)combined with aroma intensity value.The optimalextraction parameters were achieved on Rt-Wax column under the following conditions:50/30μm poly two vinyl benzene/carbon molecular sieve/poly two methyl siloxane(DVB/CAR/PDMS)solid-phase micro extraction fiber,extraction of8.0mLof sample in a20.0mL vial for40min at55℃with the addition of0.40g/mL of NaCl,20min equilibration and5mindesorption.The results showed that a total of108compounds were isolated the structures of86compounds of which wereidentified by HS-SPME-GC-O-MS,accounting for97.09%of the total volatile substances.Evaluation of OAV and aromaintensity values indicated that1-butanol3-methyl-acetate,3-methyl-1-butanol,hexanoic acid ethyl ester,2-hexenoic acidethyl ester,heptanoic acid ethyl ester,acetic acid,1-octanol,decanoic acid ethyl esterl,benzoic acid ethyl ester,pentanoicacid,acetic acid2-phenylethyl ester,hexanoic acid,benzyl alcohol,benzenepropanoic acid ethyl ester,phenylethyl alcohol,octanoic acid,and n-decanoic acid were the main aroma components.These results could provide a theoretical basis forquality control and aroma evaluation of fermented Chinese jujube wine.