天然产物研究与开发 ›› 2025, Vol. 37 ›› Issue (5): 885-894.doi: 10.16333/j.1001-6880.2025.5.010 cstr: 32307.14.1001-6880.2025.5.010

• 研究简报 • 上一篇    下一篇

化学转化法间接测定川芎药材中药效标志物藁本内酯含量的方法研究

张圆圆1,2,赵 盼2,朱芙琴1,2,潘文浩2,徐健辉2,余 琰1*,柳军玺2*   

  1. 1甘肃中医药大学药学院;2中国科学院兰州化学物理研究所 西北特色植物资源化学重点实验室 甘肃省天然药物重点实验室,兰州 730000
  • 出版日期:2025-05-28 发布日期:2025-05-26
  • 基金资助:
    甘肃省科技重大专项(21ZD2JA004);2023年度甘肃省自然科学基金(23JRRA1715)

Method study on indirect content determination of the pharmacological marker ligustilide in Chuanxiong Rhizoma by chemical transformational method

ZHANG Yuan-yuan1,2,ZHAO Pan2,ZHU Fu-qin1,2,PAN Wen-hao2,XU Jian-hui2,YU Yan1 *,LIU Jun-xi2 *   

  1. 1College of Pharmacy,Gansu University of Chinese Medicine;2Chinese Academy of Sciences Key Laboratory of Chemistry of Northwestern Plant Resources,Key Laboratory for Natural Medicine of Gansu Province,Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences,Lanzhou 730000,China
  • Online:2025-05-28 Published:2025-05-26

摘要:

通过化学转化法建立间接准确测定川芎药材中药效标志物藁本内酯含量的方法,并通过药材的HPLC-DAD特征图谱法验证该方法的准确性,该转化反应可将药材中的藁本内酯完全转化为环丙藁本,并通过对照品外标法测定反应液中环丙藁本的准确含量间接计算川芎药材中藁本内酯的含量;通过乙腈/0.1%磷酸水溶液建立梯度洗脱的HPLC-DAD方法,以洋川芎内酯I、洋川芎内酯H、阿魏酸松柏酯、洋川芎内酯A及藁本内酯指标测定川芎药材的主要苯酞类活性成分的含量,并通过特征图谱法中藁本内酯峰面积和化学转化法所得含量进行相关性分析验证化学转化法的准确性,通过线性拟合得到两种方法的线性方程(Y= 0.000 5X + 0.079 2,R = 0.996 1)支持该方法的准确性。通过51份产地川芎样本的藁本内酯的含量测定,确定川芎中藁本内酯的平均含量为1.622% ± 0.310%。本研究表明化学转化法可以准确测定川芎药材中藁本内酯的含量,通过大量川芎样本的含量测定结果可以为《中华人民共和国药典》川芎项下的定量控制指标的提高提供参考。

关键词: 川芎, 藁本内酯, 含量测定, 特征图谱法, 化学转化法

Abstract:

The aim of this study is to indirectly and accurately determine the content of ligustilide, a pharmacological marker in Chuanxiong Rhizoma, through chemical transformation method, and to validate the accuracy of this method using high-performance liquid chromatography diode array detection(HPLC-DAD) specific chromatogram method. During the chemical transformation process, the ligustilide in Chuanxiong Rhizoma can be completely converted into cyclopropyl-ligustilide. By using the reference standard external standard method, the content of cyclopropyl-ligustilide in the reaction solution can be accurately measured, thereby indirectly calculating the content of ligustilide in Chuanxiong Rhizoma. A gradient elution HPLC-DAD method was developed using acetonitrile and 0.1% phosphoric acid aqueous solution as the mobile phase, selecting senkyunolide I, senkyunolide H, coniferyl ferulate, senkyunolide A, ligustilide as indicator components to quantitatively analyze the main active components of phthalein in Chuanxiong Rhizoma. Perform correlation analysis between the peak area of ligustilide and the content obtained through chemical conversion method using specific chromatogram method to verify the accuracy of chemical conversion method. The linear equations (Y=0.000 5X+0.079 2, R=0.996 1) obtained through linear fitting support the accuracy of the chemical transformation method. By measuring the content of ligustilide in 51 samples of Ligusticum chuanxiong from different regions, this study determined that the average content of ligustilide in Chuanxiong Rhizoma was 1.622 ± 0.310%. The research results indicate that the chemical conversion method is suitable for accurately determining the content of ligustilide in Chuanxiong Rhizoma. The findings from the extensive sample analysis provide significant reference for enhancing the quantitative control standards of Chuanxiong Rhizoma in the Pharmacopoeia of the People's Republic of China.

Key words:

Chuanxiong Rhizoma, ligustilide, assay, specific chromatogram method, chemical transformational method

中图分类号:  R284.1