中国药物警戒 ›› 2023, Vol. 20 ›› Issue (9): 987-991.
DOI: 10.19803/j.1672-8629.20220735

• 基础与临床研究 • 上一篇    下一篇

超高效液相色谱-质谱联用同时测定旋覆代赭汤中15种成分含量

高乐, 王相, 麻景梅, 张泽昭, 王鑫国, 牛丽颖*   

  1. 河北中医学院,河北省中药配方颗粒技术创新中心,中药材品质评价与标准化河北省工程研究中心,河北 石家庄 050091
  • 收稿日期:2022-12-28 出版日期:2023-09-15 发布日期:2023-09-14
  • 通讯作者: *牛丽颖,女,教授·博导,中药分析与质量控制。E-mail: niuliyingyy@163.com
  • 作者简介:高乐,男,硕士,实验师,中药分析与质量控制。
  • 基金资助:
    河北省自然科学基金资助项目(H2022423335); 河北省重点研发计划(20372502D); 河北省中医药管理局项目（2020138）

Simultaneous determination of fifteen components in Xuanfudaizhe decoction by UPLC-MS/MS

GAO Le, WANG Xiang, MA Jingmei, ZHANG Zezhao, WANG Xinguo, NIU Liying*   

  1. Hebei University of Chinese Medicine, Hebei Traditional Chinese Medicine Formula Granule Engineering & Technology Innovation Center, Hebei Engineering Research Center for Quality Evaluation & Standardization of Traditional Chinese Medicine, Shijiazhuang Hebei 050091, China
  • Received:2022-12-28 Online:2023-09-15 Published:2023-09-14

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摘要： 目的 建立同时测定旋覆代赭汤中15种成分含量的超高效液相色谱-质谱联用（UPLC-MS/MS）方法。方法 采用Shim-pack GIST C18（2.1 mm × 100 mm,2.0 μm）色谱柱,流动相用乙腈-0.1%甲酸,梯度洗脱,流速0.3 mL·min-1,柱温35℃。采用ESI源,以MRM负离子模式检测。结果 甘草苷、甘草酸、甘草素、异甘草素、异甘草苷、芹糖异甘草苷、新甘草苷、绿原酸、隐绿原酸、阿魏酸、异绿原酸A、异绿原酸C、人参皂苷Rb1、人参皂苷Re和6-姜辣素在各自浓度范围内线性关系良好（r>0.998 6）,平均回收率在97.0%~103.1%,精密度、重复性、稳定性均符合要求。结论 建立的方法简单、准确性好,可为旋覆代赭汤及其制剂的质量控制提供参考。

关键词: 超高效液相色谱-质谱联用, 旋覆代赭汤, 黄酮类, 有机酸类, 皂苷类, 含量测定

Abstract: Objective To establish a method for simultaneous determination of fifteen components in Xuanfudaizhe decoction by UPLC-MS/MS. Methods The separation was performed on a Shim-pack GIST C18 column (2.1 mm × 100 mm, 2.0 μm) with acetonitrile-0.1% formic acid as the mobile phase under gradient elution at a flow rate of 0.3 mL·min-1. The column temperature was 35℃. The detection was carried out via electrospray ionization (ESI). Multiple-reaction monitoring (MRM) scanning was used for quantification in a negative ion mode. Results Liquiritin, glycyrrhizic acid, liquiritigenin, isoliquiritigeni, isoliquiritin, isoliquiritin apioside, neoliquiritin, chlorogenic acid, cryptochlorogenic acid, ferulic acid, isochlorogenic acid A, isochlorogenic acid C, ginsenoside Rb1, ginsenoside Re and 6-gingerol had good linear relationships in their respective concentration ranges (r>0.998 6). The average recovery ranged from 97.0% to 103.1%, and the precision, stability and repeatability of the method were good. Conclusion This method is simple and accurate, which can provide reference for Xuanfudaizhe decoction and its preparations.

Key words: UPLC-MS/MS, Xuanfudaizhe decoction, flavonoids, organic acids, saponins, content determination

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