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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

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为全面了解小米黄酒风味成分的构成和气味特征,优化了85μm聚丙烯酸酯(PA)、100μm聚二甲基硅氧烷(PDMS)、75μm碳分子筛(CAR)/PDMS、50/30μm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.
Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction
To comprehensively understand flavor compounds and aroma characteristics of fox-tail 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 microex-traction ( 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 com-pounds. 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.

gas chromatography-mass spectrometry ( GC-MS)headspace solid phase micro-extraction ( HS-SPME)flavor compoundsfoxtail millet wine

刘敬科、张爱霞、李少辉、赵巍、张玉宗、邢国胜

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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

石家庄制酒厂,河北 石家庄050061

气相色谱-质谱 顶空固相微萃取 风味成分 小米黄酒

现代农业产业技术体系项目河北省渤海粮仓科技示范工程项目河北省现代农业创新工程项目

CARS-06-13.5-A29HBBHLC-08F17R02

2017

色谱
中国化学会

色谱

CSTPCDCSCD北大核心
影响因子:2.171
ISSN:1000-8713
年,卷(期):2017.35(11)
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