HPLC-MS/MS测定当归六黄汤中4种不同成分的含量
投稿时间:2023-05-06  修订日期:2023-11-24  点此下载全文
引用本文:李丹,戴贤春,王芳珍,陈奕含,杨萍,刘继勇.HPLC-MS/MS测定当归六黄汤中4种不同成分的含量[J].药学实践杂志,2024,42(6):248~252,266
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作者单位E-mail
李丹 复旦大学附属肿瘤医院药剂科, 复旦大学上海医学院肿瘤学系, 上海 200032  
戴贤春 上海市质子重离子医院药剂科, 上海 201315  
王芳珍 复旦大学药学院分析测试中心, 上海 201203  
陈奕含 复旦大学药学院分析测试中心, 上海 201203  
杨萍 复旦大学药学院分析测试中心, 上海 201203  
刘继勇 复旦大学附属肿瘤医院药剂科, 复旦大学上海医学院肿瘤学系, 上海 200032
上海市质子重离子医院药剂科, 上海 201315 
liujiyong@fudan.edu.cn 
基金项目:上海市卫生健康委员会中医药传承和科技创新项目(ZYCC2019023)
中文摘要:目的 建立HPLC-MS/MS的分析方法同时测定当归六黄汤中4种主要成分黄柏碱、巴马汀、毛蕊异黄酮、阿魏酸的含量,为当归六黄汤的质量控制提供方法学参考和借鉴。方法 基于HPLC-MS/MS的分析方法,质谱检测采用ESI源MRM的正离子数据采集模式。色谱柱为Agilent Extend-C18(5 μm, 4.6 mm×250 mm),甲醇和含0.5%的甲酸水溶液进行梯度洗脱。结果 黄柏碱的线性范围为2~200 nmol/ml,巴马汀、毛蕊异黄酮、阿魏酸的线性范围均为20~2 000 nmol/ml,当归六黄汤7批样品中4种成分的含量相对稳定,其中,阿魏酸主要存在于黄柏和黄连中;黄柏碱只在黄柏中测到;毛蕊异黄酮在黄芩和黄芪中含量较高;巴马汀在黄柏和黄芪中都能检测到。结论 该方法灵敏度高,专属性好,样品的稳定性良好,能够满足中药复方定量分析的要求,可用于当归六黄汤的质量控制和评价研究。
中文关键词:当归六黄汤  黄柏碱  巴马汀  毛蕊异黄酮  阿魏酸  含量测定
 
Determination of four different components in Danggui Liuhuang decoction by HPLC-MS/MS
Abstract:Objective To establish the method of simultaneous determination of four main components of Danggui Liuhuang Decoction, including phellodendrine, palmatine, calycosin, and ferulic acid and provide reference for the quality control of Danggui Liuhuang Decoction. Methods Based on the HPLC-MS/MS analysis method, the positive ion data acquisition mode were adopted for the mass spectrometry detection and the four main components were quantified with multiple reaction monitoring mode (MRM) by ESI source. The chromatographic column was Agilent Extend-C18 (5 μm, 4.6 mm×250 mm), and gradient elution was performed with methanol and 0.5% formic acid in water. Results The linear range of phellodendrine was from 2-200 nmol/ml, and the linear range of palmatine, calycosin and ferulic acid was from 20-2 000 nmol/ml. The contents of the four components in the seven batches of Danggui Liuhuang Decoction were relatively stable, among which ferulic acid was mainly found in Phellodendrine and Coptidis; Phellodendrine was only detected in cortex phellodendri; the content of calycosin in Scutellaria baicalensis and Astragalus was higher; palmatine was detected in both Phellodendron and Astragalus. Conclusion The method had high sensitivity, good specificity and sample stability, which could meet the requirements of quantitative analysis of Traditional Chinese Medicine compounds, and could provide reference for further pharmacokinetics study on the content changes of traditional Chinese medicine compounds in biological samples.
keywords:Danggui Liuhuang decoction  phellodendron  palmatine  calycosin  ferulic acid  content determination
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