食品与发酵工业 >

2026 , Vol. 52 >Issue 16: 362 - 369

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.044829

分析与检测

基于固相萃取结合气相色谱-质谱联用法测定山西陈醋中的川芎嗪含量

  • 王梦莹 ,
  • 李国辉 ,
  • 武竹英 ,
  • 安红梅 ,
  • 杨紫欣 ,
  • 邬浩霖 ,
  • 冯迪 ,
  • 张翠英 ,
  • 王道兵 ,
  • 钟其顶
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  • 1(天津科技大学 生物工程学院,天津,300457)
    2(国家市场监督管理总局技术创新中心(轻工消费品质量安全),北京,100015)
    3(中轻技术创新中心有限公司,北京,100015)
    4(中轻检验认证(太原)有限公司,山西 太原,030400)
    5(华南理工大学 食品科学与工程学院,广东 广州,510640)
第一作者:硕士研究生(钟其顶正高级工程师和武竹英高级工程师为共同通信作者,Email:zhongqiding@163.com;zhuyingwu365@126.com)

收稿日期: 2025-10-15

  修回日期: 2026-01-07

  网络出版日期: 2026-09-10

基金资助

国家重点研发计划(2023YFF1104700);山西省重点研发计划(202402130501001);中轻集团科技项目(ZQ2021JC03)

收起

Determination of tetramethylpyrazine in Shanxi aged vinegar based on solid-phase extraction coupled with gas chromatography-mass spectrometry

  • WANG Mengying ,
  • LI Guohui ,
  • WU Zhuying ,
  • AN Hongmei ,
  • YANG Zixin ,
  • WU Haolin ,
  • FENG Di ,
  • ZHANG Cuiying ,
  • WANG Daobing ,
  • ZHONG Qiding
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  • 1(College of Bioengineering, Tianjin University of Science and Technology, Tianjin 300457, China)
    2(Technology Innovation Center of Light Industrial Consumer Goods Quality and Safety for State Administration for Market Regulation, Beijing 100015, China)
    3(Sinolight Technology Innovation Centre Co.Ltd, Beijing 100015, China)
    4(Sinolight Inspection and Certification (Taiyuan) Co.Ltd., Taiyuan 030400, China)
    5(School of Food Science and Engineering, South China University of Technology, Guangzhou 510640, China)

Received date: 2025-10-15

  Revised date: 2026-01-07

  Online published: 2026-09-10

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摘要

该研究建立了应用固相萃取(solid-phase extraction, SPE)结合气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)快速测定食醋中川芎嗪(tetramethylpyrazine, TMP)含量的分析方法。样品经Poly-Sery HLB Pro SPE小柱净化后,采用GC-MS外标法定量。该方法重复性及仪器精密度的相对标准偏差(relative standard deviation, RSD)均小于3%,加标回收率为96.90%～100.79%。TMP在0.1～100 mg/L质量浓度内线性关系良好,相关系数r2>0.999 9。方法的检出限为0.309 μg/L,定量限为1.031 μg/L。该方法定量准确、操作简便、灵敏度高,适用于食醋中TMP的测定。此外,对地理标志产品山西老陈醋和非地理标志陈醋样品分析,结果表明两类产品中TMP含量差异显著。

关键词： 川芎嗪; 山西陈醋; 固相萃取; 气相色谱-质谱联用; 特征指标

本文引用格式

王梦莹 , 李国辉 , 武竹英 , 安红梅 , 杨紫欣 , 邬浩霖 , 冯迪 , 张翠英 , 王道兵 , 钟其顶 . 基于固相萃取结合气相色谱-质谱联用法测定山西陈醋中的川芎嗪含量[J]. 食品与发酵工业, 2026 , 52(16) : 362 -369 . DOI: 10.13995/j.cnki.11-1802/ts.044829

Abstract

This study established a rapid method for quantitative determination of tetramethylpyrazine (TMP) in vinegar by using solid-phase extraction (SPE) coupled with gas chromatography-mass spectrometry (GC-MS).The vinegar samples were purified by Poly-Sery HLB Pro SPE solid phase extraction column, and then quantified by external standard method with GC-MS.The method demonstrated good repeatability and instrument precision, with RSDs of less than 3%, and the recovery rates were 96.90%-100.79%.Excellent linearity for TMP was achieved over the concentration range of 0.1-100 mg/L, with the correlation coefficient (r2) of 0.999 9.In addition, the detection limit (LOD) was 0.309 μg/L and the quantification limit (LOQ) was 1.031 μg/L.This method was accurate, simple to operate, and highly sensitive, making it suitable for TMP determination in vinegar.Furthermore, an analysis of the tetramethylpyrazine (TMP) content in geographical indication (GI) Shanxi aged vinegar and non-GI vinegar samples was conducted.The results indicated a significant difference in the TMP content between the two product categories.

Key words： tetramethylpyrazine; Shanxi aged vinegar; solid phase extraction; gas chromatography-mass spectrometry; characteristic indicators

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