食品科学 ›› 2021, Vol. 42 ›› Issue (20): 114-119.doi: 10.7506/spkx1002-6630-20200805-071

• 成分分析 • 上一篇    下一篇

LLE-GC-MS-SIM检测白酒中9 种微量功能成分

史改玲,郭莹,李景辉,王国明,尹翠娟,李秋志,张翠英   

  1. (1.工业发酵微生物教育部重点实验室,天津市工业微生物重点实验室,天津科技大学生物工程学院,天津 300457;2.承德避暑山庄企业集团股份有限公司,河北 承德 067500)
  • 出版日期:2021-10-25 发布日期:2021-11-12
  • 基金资助:
    国家自然科学基金面上项目(31471724);天津市科委自然基金重点项目(14JCZDJC32900)

Determination of Nine Trace Functional Components in Chinese Baijiu by Liquid-liquid Extraction Coupled to Gas Chromatography-Mass Spectrometry-Selective Ion Monitoring

SHI Gailing, GUO Ying, LI Jinghui, WANG Guoming, YIN Cuijuan, LI Qiuzhi, ZHANG Cuiying   

  1. (1. Key Laboratory of Industrial Fermentation Microbiology, Ministry of Education, Tianjin Industrial Microbiology Key Laboratory,College of Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, China; 2. Chengde Bishu Villas Enterprise Group Co. Ltd., Chengde 067500, China)
  • Online:2021-10-25 Published:2021-11-12

摘要: 应用液液萃取(liquid-liquid extraction,LLE)结合气相色谱-质谱-选择离子扫描(gas chromatography-mass spectrometry-selective ion monitoring,GC-MS-SIM)技术检测20 种白酒中D-柠檬烯、对伞花烃、叶绿醇、4-甲基愈创木酚、4-乙基愈创木酚、麝香草酚、异丁香酚、四甲基吡嗪及亚油酸乙酯含量。该方法回收率在81.80%~109.30%之间,精密度均小于6.00%;检测范围内,线性关系良好(R2>0.999 0),检出限和定量限分别为0.17~0.91 μg/L和0.58~3.04 μg/L。LLE-GC-MS-SIM法对9 种功能成分的定量检测结果表明,3 种萜烯类物质在浓香型酒样中含量较高,且山庄酒厂酒样含量普遍高于市售酒样;芝麻香型白酒中酚类物质含量最高,其中酒样W09中4 种酚类物质质量浓度高达4 301.61 μg/L;四甲基吡嗪在酱香型酒样中质量浓度为2 379.65~2 985.09 μg/L,远高于芝麻香型酒样的1 116.80~1 309.66 μg/L及浓香型酒样的245.40~555.76 μg/L;亚油酸乙酯在不同酒样中含量差异较大,除市售酒样W17、W19和W20外,其余酒样质量浓度为1 951.96~7 183.35 μg/L。

关键词: 中国白酒;微量功能成分;液液萃取;气相色谱-质谱-选择离子扫描

Abstract: Totally nine volatile trace components in 20 samples of different kinds of Chinese Baijiu were analyzed by liquid-liquid extraction (LLE) combined with gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM). The average recoveries of the developed method were in the range of 81.80%–109.30%, with a precision (relative standard deviation, RSD) of less than 6.00%. Excellent linearity was observed in the tested concentration range (R2 > 0.999 0). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.17–0.91 and 0.58–3.04 μg/L, respectively. The results showed that among the nine functional compounds, three terpenes had higher concentrations in Nongxiangxing Baijiu, and their concentrations in the Baijiu samples from a producer in Chengde, Hebei were higher than those in other samples examined. Four phenolic compounds had the highest concentrations in Zhima-flavor Baijiu, and the total amount of phenolics was 4 301.61 μg/L in sample W09. The concentration of tetramethylpyrazine in Jiang-flavor Baijiu was 2 379.65–2 985.09 μg/L, much higher than that in Zhima-flavor Baijiu (1 116.80–1 309.66 μg/L) and Nongxiangxing Baijiu (245.40–555.76 μg/L). The concentration of linoleic acid ethyl ester significantly varied in the range of 1 951.96–7 183.35 μg/L among different samples expect for W17, W19 and W20.

Key words: Chinese Baijiu; trace functional compounds; liquid-liquid extraction; gas chromatography-mass spectrometry-selective ion monitoring

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