食品科学 ›› 2017, Vol. 38 ›› Issue (18): 73-79.doi: 10.7506/spkx1002-6630-201718012

• 成分分析 • 上一篇    下一篇

涡旋辅助液液微萃取结合GC-MS法检测67 种白酒中四甲基吡嗪、4-甲基愈创木酚4-乙基愈创木酚

孙啸涛,王宗元,刘淼,敖灵,孙宝国,孙金沅,郑福平,黄明泉,李贺贺   

  1. (1.天津科技大学食品工程与生物技术学院,天津 300457;2.食品质量与安全北京实验室(北京工商大学),北京 100048;3.泸州老窖股份有限公司,四川?泸州 646000)
  • 出版日期:2017-09-25 发布日期:2017-09-04
  • 基金资助:
    国家自然科学基金青年科学基金项目(31601556);“十三五”国家重点研发计划重点专项(2016YFD0400501); 四川省科技计划项目(2017JZ0012)

Determination of Tetramethylpyrazine-4-Methyl Guaiacol and 4-Ethyl Guaiacol in 67? Chinese Baijiu Samples by Vortex Assisted Liquid-Liquid Microextration Combined with Gas Chromatography-Mass Spectrometry

SUN Xiaotao, WANG Zongyuan, LIU Miao, AO Ling, SUN Baoguo, SUN Jinyuan, ZHENG Fuping, HUANG Mingquan, LI Hehe   

  1. (1.College of Food Engineering and Biotechnology, Tianjin University of Science and Technology, Tianjin 300457, China; 2. Beijing Laboratory for Food Quality and Safety, Beijing Technology & Business University (BTBU), Beijing 100048, China; 3. Luzhou Laojiao Co. Ltd., Luzhou, Sichuan 646000, China)
  • Online:2017-09-25 Published:2017-09-04

摘要: 采用涡旋辅助液液微萃取结合气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)法对67?种白酒中四甲基吡嗪、4-甲基愈创木酚和4-乙基愈创木酚进行检测。酒样经二氯甲烷提取,涡旋辅助萃取1?min,6?000?r/min离心5?min,然后采用GC-MS进行分析。结果表明,四甲基吡嗪、4-甲基愈创木酚和4-乙基愈创木酚分别在质量浓度为0.5~2?500、1.0~2?500、1.0~2?500?μg/L的范围内具有较好的线性关系(R2>0.99);检出限分别为0.25、0.5、0.5?μg/L;不同添加水平的平均回收率为80.1%~88.0%。对67?种白酒含量分析表明,所有样本都含有四甲基吡嗪,含量范围为1.5~2?434.3?μg/L;51?种样本中含有4-甲基愈创木酚,含量范围为2.8~1?709.0?μg/L;53?种样本中含有4-乙基愈创木酚,含量范围为1.3~1?167.5?μg/L。白酒酿造原料、工艺的差异可能是造成其健康因子含量不同的潜在因素。

关键词: 白酒, 四甲基吡嗪, 4-甲基愈创木酚, 4-乙基愈创木酚, 涡旋辅助液液微萃取(VALLME)法

Abstract: Tetramethylpyrazine, 4-methyl guaiacol and 4-ethyl guaiacol in 67 Chinese Baijiu samples were detected by vortex assisted liquid-liquid microextration (VALLME) combined with gas chromatography-mass spectrometry (GC-MS). The analytes were extracted with CH2Cl2, using a vortex agitator for 1?min, and then centrifuged at 6 000?r/min for 5?min. After that, the CH2Cl2 phase was directly injected into GC-MS for analysis. The results indicated that the calibration curves for the three analytes displayed a good linearity (R2 > 0.99) in the ranges of 0.5–2 500, 1.0–2 500, and 1.0–2 500?μg/L, respectively. The limits of detection (LODs) for tetramethylpyrazine, 4-methylguaiacol and 4-ethyl guaiacol were 0.25, 0.5 and 0.5?μg/L, respectively. The recoveries were in the range of 80.1%–88.0%. The method was successfully employed to detect the analytes in 67? Chinese Baijiu samples and the results showed that all the samples contained 1.5–2 434.3?μg/L tetramethylpyrazine, of which 51 contained 2.8–1 709.0?μg/L 4-methylguaiacol, and 53 contained 1.3–1 167.5?μg/L 4-ethyl guaiacol. The differences in the contents of the health-beneficial ingredients in Chinese Baijiu may be related to the raw materials and manufacturing process.

Key words: Baijiu, tetramethylpyrazine, 4-methyl guaiacol, 4-ethyl guaiacol, vortex assisted liquid-liquid microextration (VALLME)

中图分类号: