食品科学 ›› 2011, Vol. 32 ›› Issue (22): 179-183.doi: 10.7506/spkx1002-6630-201122036

• 分析检测 • 上一篇    下一篇

气相色谱-质谱结合吸附萃取法测定陈酿黄酒挥发性香气物质

于海燕1,张 妮2,朱建才1   

  1. 1.上海应用技术学院香料香精技术与工程学院 2.华东理工大学生物工程学院
  • 出版日期:2011-11-25 发布日期:2011-11-11
  • 基金资助:
    教育部高等学校全国优秀博士论文作者资助专项(201059);上海市自然科学基金项目(10ZR1429600)

Determination of Volatiles in Chinese Rice Wine by Sorptive Extraction Coupled with Gas Chromatography-Mass Spectrometry

YU Hai-yan1,ZHANG Ni2,ZHU Jian-cai1   

  1. (1. School of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 200233, China; 2. School of Biotechnology, East China University of Science and Technology, Shanghai 200237, China)
  • Online:2011-11-25 Published:2011-11-11

摘要: 建立吸附法进行香气提取、气相色谱-质谱法测定不同酒龄黄酒中挥发性香气物质的方法。对比分析固相微萃取和搅拌棒吸附萃取对黄酒香气提取的效果,获得优化的香气提取方法。结果表明:采用搅拌棒吸附萃取-气相色谱-质谱法测定黄酒挥发性香气物质的平均相对标准偏差为11.47%,回收率为88.6%~92.3%,说明所建方法稳定;采用搅拌棒吸附萃取-气相色谱-质谱法共测得60种挥发性香气物质,其中15种醇类物质、25种酯类、6种醛类和5种酸类物质;随酒龄增加,乙醇含量逐渐减少,而11种酯类、1种醇类、1种酮类和1种醛类含量逐渐增加,随陈酿时间增加,部分醇、醛类物质被催化氧化成有机酸,酸的增加促进了酯化反应。搅拌棒吸附萃取-气相色谱-质谱法具有前处理简单快捷、重复性好等优点,可为黄酒香气分析提供准确可靠的数据。

关键词: 黄酒, 搅拌棒吸附萃取, 固相微萃取, 气相色谱-质谱

Abstract: A method was developed for the determination of volatiles in Chinese rice wine with different aging times by gas chromatography-mass spectrometry (GC-MS) with sorptive extraction. Solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE) were compared to select the best extraction method among the two. Compared with SPME, SBSE resulted in a higher-fold enrichment and a lower limit of detection. The average relative standard deviation (RSD) of the developed SBSE/GC-MS method (6 parallel determinations) was 11.47% and the recoveries for isobutyl alcohol, furfural and ethyl acetate were in the range of 88.6%-92.3%, suggesting its good stability. Sixty volatiles were identified and quantified, including 15 alcohols, 25 esters, 6 aldehydes and 5 acids, and others. With increasing aging time, ethanol concentration showed a gradual decrease, while the concentrations of 11 esters, 1 alcohol, 1 ketone and 1 aldehyde gradually increased. These changes may be caused by the oxidation of alcohols and aldehydes into acids followed by the esterification of acids and alcohols during storage. In conclusion, SBSE/GC-MS is a reliable method allowing the determination of volatiles in Chinese rice wine.

Key words: Chinese rice wine, stir bar sorptive extraction (SBSE), solid phase microextraction (SPME), gas chromatography-mass spectrometry (GC-MS)

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