中国药物警戒 ›› 2026, Vol. 23 ›› Issue (1): 88-94.
DOI: 10.19803/j.1672-8629.20250577

• 基础与临床研究 • 上一篇    下一篇

止嗽化痰丸中马兜铃去籽碱制减毒研究及其质量控制

刘素彦1, 李春英1, 易艳1, 赵雍1, 韩佳寅1, 潘辰1, 张宇实1, 余渊2, 刘青3, 梁爱华1,*   

  1. 1中国中医科学院中药研究所,北京 100700;
    2贵州中医药大学药学院,贵州 贵阳 550025;
    3贵州医科大学药学院,贵州 贵阳 561113
  • 收稿日期:2025-08-18 出版日期:2026-01-15 发布日期:2026-01-15
  • 通讯作者: *梁爱华,女,博士,研究员,中药毒理学。E-mail: ahliang@icmm.ac.cn
  • 作者简介:刘素彦,女,博士,助理研究员,中药毒理学。
  • 基金资助:
    国家自然科学基金资助项目（82192913、82174073、82304851、82304861）; 贵州省揭榜挂帅项目（筑科[2024]-6-3号）

Seed-Removal and Alkaline-Treatment of Aristolochia contorta Bge. in Zhisou Huatan Pills and Quality Control: a Detoxification Study

LIU Suyan1, LI Chunying1, YI Yan1, ZHAO Yong1, HAN Jiayin1, PAN Chen1, ZHANG Yushi1, YU Yuan2, LIU Qing3, LIANG Aihua1,*   

  1. 1Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences, Beijing 100700, China;
    2College of Pharmacy, Guizhou University of Traditional Chinese Medicine, Guiyang Guizhou 550025, China;
    3School of Pharmaceutical Sciences, Guizhou Medical University, Guiyang Guizhou 561113, China
  • Received:2025-08-18 Online:2026-01-15 Published:2026-01-15

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摘要： 目的 通过测定马兜铃炮制前后及止嗽化痰丸中5种马兜铃酸类物质的含量,考察去籽碱制对马兜铃及止嗽化痰丸的减毒效果,为其质量控制提供借鉴。方法 采用ACQUITY UPLC BEH C18色谱柱（2.1 mm×50 mm,1.7 μm,Waters）,以甲醇和水（含5.0 mmol·L-1醋酸铵和0.1%甲酸）为流动相进行梯度洗脱。采用电喷雾离子源（ESI）,正离子模式下多反应监测方式（MRM）,建立同时测定5种马兜铃酸类成分（AAⅠ、AAⅡ、AAⅢa、AAⅣa和ALⅠ）的高效液相色谱-三重四极杆质谱（UPLC-MS/MS）定量分析方法。结果 马兜铃药材中AAⅠ、AAⅡ、AAⅢa、AAⅣa及ALⅠ的含量分别在573.12~880.72 μg·g-1、37.12~97.02 μg·g-1、236.68~461.83 μg·g-1、376.60~414.37 μg·g-1和262.58~393.83 μg·g-1。去籽碱制马兜铃中AAⅡ含量低于方法检测限;能够检测到AAⅠ、AAⅢa及AAⅣa,但是其信号低于相应的定量限;ALⅠ的含量在25.15~35.29 μg·g-1。止嗽化痰丸样品中AAⅠ、AAⅡ、AAⅢa和AAⅣa含量低于方法检测限,ALⅠ含量在0.87~0.97 μg·g-1。结论 去籽碱制能够显著降低马兜铃中AAⅠ、AAⅡ、AAⅢa、AAⅣa和ALⅠ的含量。10批止嗽化痰丸中未检出AAⅠ。建立的UPLC-MS/MS定量检测方法,专属性强、灵敏度高、重复性好,可为止嗽化痰丸的质量控制提供参考。

关键词: 去籽碱制, 马兜铃, 止嗽化痰丸, 马兜铃酸, 高效液相色谱-三重四极杆质谱, 质量控制

Abstract: Objective To investigate the detoxification of Aristolochia contorta Bge. in Zhisou Huatan pills via seed-removal and al kali-treatment based on quantitative determination of five aristolochic acid analogues in order to provide a reference for quality control. Methods The separation was performed on an ACQUITY UPLC BEH C18 column (2.1 mm×50 mm, 1.7 μm) with methanol-water (containing 0.1% formic acid and 5.0 mmol·L-1 ammonium acetate) as the mobile phases at a flow rate of 0.3 mL·min-1. The multiple reaction monitoring mode (MRM) was used in positive ion acquisition. The established method was employed to quantitatively detect the contents of five aristolochic acid analogues in five batches of Aristolochia contorta Bge., ten batches of seed-removal Aristolochia contorta Bge., seed-removed and alkaline-processed Aristolochia contorta Bge., and in Zhisou Huatan pills. Results The contents of AAⅠ, AAⅡ, AAⅢa, AAⅣa, and ALⅠin Aristolochia contorta Bge. ranged from 573.12 to 880.72 μg·g-1, 37.12 to 97.02 μg·g-1, 236.68 to 461.83 μg·g-1, 376.60 to 414.37 μg·g-1 and 262.58 to 393.83 μg·g-1, respectively. The content of AAⅡ was below the detection limit in seed-removed and alkaline-processed Aristolochia contorta Bge. but AAⅠ, AAⅢa, and AAⅣa could still be detected, and their concentrations were below the limit of quantification. The content of ALⅠ ranged from 25.15 to 35.29 μg·g-1. AAⅠ, AAⅡ, AAⅢa, or AAⅣa were detected in Zhisou Huatan pills, and the content of ALⅠ ranged from 0.87 to 0.97 μg·g-1. Conclusion Seed-removal and alkali-treatment can significantly reduce the contents of AAⅠ, AAⅡ, AAⅢa, AAⅣa, and ALⅠ in Aristolochia contorta Bge. AAⅠ is not detected in Zhisou Huatan pills. The established UPLC-MS/MS method has a high specificity, high sensitivity, and good repeatability, which can provide a reference for quality control of Zhisou Huatan pills.

Key words: Seed-Removal and Alkali-Treatment, Aristolochia contorta Bge., Zhisou Huatan Pills, Aristolochic Acids, UPLC-MS/MS, Quality Control

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