HS-SPME-GC-O-MS联用法分析红枣发酵饮料易挥发性成分条件的优化

以红枣发酵饮料为研究对象,利用顶空固相微萃取和气相色谱-嗅闻-质谱联用法分析其易挥发性成分并对其进行了分析,对影响固相微萃取操作条件的萃取头、萃取温度、萃取时间、样品用量、平衡时间和解吸时间进行系统的优化,旨在建立一种分析红枣发酵饮料易挥发性成分的方法,并通过嗅闻检测结合气味活度值和香气强度值确定红枣发酵饮料的特征风味成分,采用草酸二乙酯做内标对特征风味成分进行了含量测定。结果表明:选用50/30μm DVB/CAR/PDMS固相微萃取头、Rtx-WAX色谱柱、样品用量8.0 m L/20.0 m L样品瓶、加盐量3.00 g、萃取时间70 min、萃取温度70℃、平衡时间20 min、解吸时间3 min,分析红枣发酵饮料易挥发性成分,共检出114种组分,确定结构96种,占总易挥发性成分总量的98.86%;气味活度值及香气强度值分析结果表明:乙酸乙酯、戊酸乙酯、己酸乙酯、2-辛酮、2-十一酮、乙酸-2-苯乙酯、苯丙酸乙酯、6-甲基-5-庚烯-2-酮、苯甲醛和3-羟基-2-丁酮为红枣发酵饮料的特征风味成分。 

Optimization of volatile compounds in Chinese jujube fermented beverages by headspace solid phase micro- extraction and gas chromatography- olfactometry- mass spectrometry

The volatile compounds in Chinese jujube fermented bverages were analyzed by HS- SPME and GC- O- MS.Affecting the operation of HS- SPME experimental conditions of extraction head,extraction temperature,extraction time,sample amount,equilibrium time and desorption time were optimized,it is in order to establish a method of analysis of volatile components in Chinese jujube fermented beverages,and the contribution of the main components to the overall aroma of Chinese jujube fermented beverages was evaluated by odor activity value( OAV) combined with aroma intensity value with diethyl oxalate as internal standard substances.The results indicated that the optimal extraction performance analyzing Chinese jujube fermented beverages volatile components was 50 /30 μm poly two vinyl benzene / carbon molecular sieve / poly two methyl siloxane( DVB /CAR / PDMS) solid-phase micro extraction head,Rtx-WAX column,8.0 m L of sample add salt at 3 g with extracting at 70 ℃ for70 minutes,20 minutes equilibrium time and 3 minutes desorption time.The results showed that through the analysis of HS-SPME- GC-O-MS,a total of 114 compounds were isolated,and the structure of 96 in them were identified,accounting for 98.86% of the total volatile substances Evaluation of OAV and aroma intensity values showed that ethyl acetate,pentanoic acid ethyl ester,ethyl hexanoate,2-Nonanone,2- Undecanone,2- phenyl ethyl acetate,Benzoic acid ethyl ester,6- methyl- 5- hepten- 2- one,benzaldehyde and 3-Hydroxy-2-butanone was the main aroma components of Chinese jujube fermented beverages.