色谱

色谱 ›› 2019, Vol. 37 ›› Issue (11): 1215-1220.DOI: 10.3724/SP.J.1123.2019.04033

• 研究论文 • 上一篇    下一篇

气相色谱-三重四极杆质谱法同时测定巴氏杀菌乳中9种香精成分

刘通1, 王玉娇1,2, 王秀娟1, 崔东伟1,3, 张峰1   

  1. 1.中国检验检疫科学研究院食品安全研究所, 北京 100176;
    2.天津科技大学生物工程学院, 天津 300000;
    3.中国医科大学药学院, 沈阳 110122
  • 收稿日期:2019-04-21 出版日期:2019-11-08 发布日期:2020-12-11
  • 通讯作者: 张峰.E-mail:fengzhang@126.com.
  • 基金资助:
    国家重点研发计划（2017YFC1601600，2018YFC1603606）；国家高层次人才特殊支持计划（检科2019-006）.

Simultaneous determination of nine flavor compounds in pasteurized milk by gas chromatography- triple quadrupole mass spectrometry

LIU Tong1, WANG Yujiao1,2, WANG Xiujuan1, CUI Dongwei1,3, ZHANG Feng1   

  1. 1. Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China;
    2. College of Bioengineering, Tianjin University of Science and Technology, Tianjin 300000, China;
    3. School of Pharmacy, China Medical University, Shenyang 110122, China
  • Received:2019-04-21 Online:2019-11-08 Published:2020-12-11
  • Supported by:
    National Key Research and Development Program (Nos. 2017YFC1601600, 2018YFC1603606); National Special Support Plan for High-level Talents (No. Jianke 2019-006).

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摘要： 建立了气相色谱-三重四极杆质谱（GC-MS/MS）同时检测巴氏杀菌乳中9种香精成分（二氢香豆素、香兰素、香豆素、乙基香兰素、甲基香兰素、7-甲基香豆素、7-甲氧基香豆素、7-乙氧基-4甲基香豆素和环香豆素）的分析方法。巴氏杀菌乳样品用乙醇溶液萃取，低温涡旋离心，取上清液过0.22 μm滤膜，以DB-5MS色谱柱分离，在MRM模式下测定，基质曲线外标法定量。实验结果表明，9种香精成分在1~200 μg/L范围内呈良好线性，线性相关系数（R2）均大于0.997，方法的检出限为0.002~0.1 μg/kg，定量限为0.001~2 μg/kg，平均回收率为90.3%~110.6%，日内、日间精密度均小于10%。该方法前处理简单快速，检测准确度和灵敏度高，可用于巴氏杀菌乳中9种香精成分的同时检测。

关键词: 气相色谱-三重四极杆质谱, 香精成分, 巴氏杀菌乳

Abstract: A gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) method was established for the simultaneous determination of nine flavor compounds (hydrocoumarin, vanillin, coumarin, ethyl vanillin, methyl vanillin, 7-methylcoumarin, 7-methyoxycoumarin, 7-ethoxy-4-mrthyl coumarin, pyranocoumarin) in pasteurized milk. The samples were extracted with ethanol and subjected to whirlpool oscillation. After centrifugation, the supernatant was filtered through a membrane, and the components were separated on a DB-5MS column. The nine analytes were detected by GC-MS/MS in the multiple reaction monitoring (MRM) mode and quantified by a matrix-matched external standard method. Good linearities in the range of 1-200 μg/L were observed for the nine flavor compounds. The linear correlation coefficients (R2) were greater than 0.997. The limits of detection and limits of quantification were 0.002-0.1 μg/kg and 0.001-2 μg/kg, respectively. The average recoveries were 90.3%-110.6%. Both the intra-day and inter-day RSDs were less than 10%. The developed method is simple, rapid, accurate and sensitive, and can be used for the simultaneous determination of the nine flavor compounds in pasteurized milk.

Key words: gas chromatography-tandem mass spectrometry (GC-MS/MS), flavor compounds, pasteurized milk

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