顶空固相微萃取-气相色谱-质谱法测定小米黄酒风味成分

doi:10.3724/SP.J.1123.2017.07012

色谱

顶空固相微萃取-气相色谱-质谱法测定小米黄酒风味成分

刘敬科¹, 张爱霞¹, 李少辉¹, 赵巍¹, 张玉宗¹, 邢国胜²

1. 河北省农林科学院谷子研究所, 国家谷子改良中心, 河北省杂粮研究实验室, 河北石家庄 050035;
2. 石家庄制酒厂, 河北石家庄 050061

收稿日期:2017-07-14 出版日期:2017-11-08 发布日期:2014-01-17
通讯作者: 刘敬科,Tel:(0311)87670703,E-mail:liujingke79@163.com
基金资助:
现代农业产业技术体系项目（CARS-06-13.5-A29）；河北省渤海粮仓科技示范工程项目（HBBHLC-08）；河北省现代农业创新工程项目（F17R02）.

Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction

LIU Jingke¹, ZHANG Aixia¹, LI Shaohui¹, ZHAO Wei¹, ZHANG Yuzong¹, XING Guosheng²

1. Institute Millet Crops of Hebei Academy of Agriculture and Forestry, National Millet Improvement Center of China, Cereal Crops Research Laboratory of Hebei Province, Shijiazhuang 050035, China;
2. Shijiazhuang Wine Factory, Shijiazhuang 050061, China

Received:2017-07-14 Online:2017-11-08 Published:2014-01-17
Supported by:
Modern Agricultural Industry Technology System (No. CARS-06-13.5-A29); Hebei Provincial Bo Sea Granary the Scientific and Technological Demonstration Project (No. HBBHLC-08); Hebei Provincial Innovation of Modern Agricultural Project (No. F17R02).

摘要/Abstract

摘要：

为全面了解小米黄酒风味成分的构成和气味特征，优化了85 μm聚丙烯酸酯（PA）、100 μm聚二甲基硅氧烷（PDMS）、75 μm碳分子筛（CAR）/PDMS、50/30 μm二乙烯基苯（DVB）/CAR/PDMS萃取头提取小米黄酒风味成分的条件，采用顶空固相微萃取（headspace solid phase microextraction，HS-SPME）-气相色谱-质谱法（GC-MS）对风味成分进行定性、定量分析，并计算气味活性值（odor active value，OAV），同时利用OAV分析风味成分的气味特征和气味强度。结果显示：不同萃取头的最优萃取条件为样品量8 mL、萃取时间40 min、萃取温度60℃、NaCl添加量1.5 g。小米黄酒风味成分由醇、酯、含苯化合物、烃、酸、醛、酮、烯、酚和杂环类化合物构成，醇为主要风味成分。通过OAV确定了苯乙醇、苯乙烯、2-甲基萘、1-甲基萘、苯甲醛、苯乙醛、2-甲氧基-苯酚为小米黄酒气味特征成分，苯基乙醇、苯乙醛对气味贡献最大。PA和PDMS萃取头分别对极性和非极性化合物具有较好的吸附效果，CAR/PDMS和DVB/CAR/PDMS萃取头对中等极性化合物具有较好的吸附效果。该研究全面了解了小米黄酒风味成分的构成，为其产品开发及品质控制提供理论了依据。

关键词: 顶空固相微萃取, 风味成分, 气相色谱-质谱, 小米黄酒

Abstract: To comprehensively understand flavor compounds and aroma characteristics of foxtail millet wine, extraction conditions were optimized with 85 μm polyacrylate (PA), 100 μm polydimethylsiloxane (PDMS), 75 μm carboxen (CAR)/PDMS and 50/30 μm divinylbenzene (DVB)/CAR/PDMS fibers. The flavor compounds in foxtail millet wine were investigated by gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid phase microextraction (HS-SPME), and the odor characteristics and intensity were analyzed by odor active values (OAVs). The samples of 8 mL were placed in headspace vials with 1.5 g NaCl, then the headspace vials were heated at 60℃ for 40 min. Using HS-SPME with different fibers, a total of 55 flavor compounds were identified from the samples, including alcohols, esters, benzene derivatives, hydrocarbons, acids, aldehydes, ketones, terpenes, phenols and heterocycle compounds. The main flavor compounds were alcohols compounds. According to their OAVs, phenylethyl alcohol, styrene, 1-methyl-naphthalene, 2-methyl-naphthalene, benzaldehyde, benzeneacetaldehyde and 2-methoxy-phenol were established to be odor-active compounds. Phenylethyl alcohol and benzeneacetaldehyde were the most prominent odor-active compounds. PA and PDMS fibers had good extraction effect for polar and nonpolar compounds, respectively. CAR/PDMS and DVB/CAR/PDMS provided a similar compounds profile for moderate polar compounds. This research comprehensively determined flavor compounds of foxtail millet wine, and provided theoretical basis for product development and quality control.

Key words: flavor compounds, foxtail millet wine, gas chromatography-mass spectrometry (GC-MS), headspace solid phase microextraction (HS-SPME)

中图分类号:

O658

刘敬科, 张爱霞, 李少辉, 赵巍, 张玉宗, 邢国胜. 顶空固相微萃取-气相色谱-质谱法测定小米黄酒风味成分[J]. 色谱, DOI: 10.3724/SP.J.1123.2017.07012.

LIU Jingke, ZHANG Aixia, LI Shaohui, ZHAO Wei, ZHANG Yuzong, XING Guosheng. Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction[J]. Chinese Journal of Chromatography, DOI: 10.3724/SP.J.1123.2017.07012.

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顶空固相微萃取-气相色谱-质谱法测定小米黄酒风味成分

Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction

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