色谱

色谱 ›› 2019, Vol. 37 ›› Issue (10): 1036-1041.DOI: 10.3724/SP.J.1123.2019.01055

• 特别策划：固相萃取和QuEChERS应用专栏 • 上一篇    下一篇

QuEChERS与液相色谱-串联质谱联用检测中药、调味品及外敷药物中去甲乌药碱的含量

王晗1, 汤一铸2, 赵晓亚1, 叶诚1, 郭少飞1, 罗静1, 熊露1, 曹维1, 吴建安1, 王鹏1   

  1. 1.武汉海关技术中心, 湖北 武汉 430050;
    2.湖北省体育科学研究院, 湖北 武汉 430205
  • 收稿日期:2019-01-31 出版日期:2019-10-08 发布日期:2020-12-11
  • 通讯作者: 王鹏,Tel:(027)58906080,E-mail:pengwwang@foxmail.com.
  • 基金资助:
    国家重点研发计划（2018YFC1603500）；湖北省体育局重点领域研究课题（2018A009）.

Determination of higenamine in Chinese herbal medicine, condiments, and topical medicine by QuEChERS combined with liquid chromatography-tandem mass spectrometry

WANG Han1, TANG Yizhu2, ZHAO Xiaoya1, YE Cheng1, GUO Shaofei1, LUO Jing1, XIONG Lu1, CAO Wei1, WU Jian'an1, WANG Peng1   

  1. 1. Technology Center of Wuhan Customs, Wuhan 430050, Hubei;
    2. Hubei Institute of Sport Science, Wuhan 430205, Hubei
  • Received:2019-01-31 Online:2019-10-08 Published:2020-12-11
  • Supported by:
    the National Key Research and Development Program of China (No. 2018YFC1603500); the Key Research Subject of Hubei Sport Bureau (No. 2018A009).

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摘要： 针对中药材、调味品及外敷药物中的去甲乌药碱，建立了一种基于QuEChERS前处理与液相色谱-串联质谱（LC-MS/MS）联用的检测新方法。样品经甲酸-乙醇提取、QuEChERS吸附剂净化后，样品溶液引入LC-MS/MS进行分析，在多反应监测模式下检测。该方法的检出限为0.03 ng/g，线性范围为0.10~100 ng/g，精密度为4.33%（0.50 ng/g，n=7）。采用所建立的方法对市售的13种中药、4种调味料及1种藏药贴膏中的去甲乌药碱含量进行了检测，在干荷叶、干莲子、山药、玉竹、淮山、花椒、桂皮及骨痛贴膏中检出去甲乌药碱，其含量分别为9667.6、1183.8、21.5、8.2、8.5、148.6、21.3、173.3 μg/kg。对花椒和桂皮进行加标回收试验，回收率在92.6%~109.8%之间，表明所建立的方法具有良好的准确性。综上，该方法具有快速、简便、可靠、可批处理的优点。

关键词: QuEChERS, 液相色谱-串联质谱, 去甲乌药碱, 中药, 调味品

Abstract: A method combining QuEChERS with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of higenamine in Chinese herbal medicine, condiments, and topical medicine. The sample was subjected to extraction using a formic acid-ethanol mixture, followed by purification of the QuEChERS sorbents; then, the extraction solution was introduced into the LC-MS/MS system for detection in multiple reaction monitoring (MRM) mode. Under the optimal conditions, the detection limit of the developed method was 0.03 ng/g, and the linear range was 0.10-100 ng/g with a relative standard deviation (RSD) of 4.33% (0.5 ng/g, n=7). The method was then applied to the determination of higenamine in 13 kinds of Chinese herbal medicine, four kinds of condiments, and a topical medicine. Higenamine was detected in dried lotus leaf, dried lotus seed, Chinese yam, Yuzhu, Yam, Sichuan pepper, Cassia, and the topical medicine at 9667.6, 1183.8, 21.5, 8.2, 8.5, 148.6, 21.3, and 173.3 μg/kg, respectively. The recoveries of higenamine in Sichuan pepper and cassia was 92.6%-109.8%. In conclusion, the method is fast, simple, reliable, and suitable for use in batch operation.

Key words: QuEChERS, liquid chromatography-tandem mass spectrometry (LC-MS/MS), higenamine, Chinese herbal medicine, condiments

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