RP-HPLC-DAD法同时测定毛冬青根中4种三萜皂苷和2种木脂素的含量

doi:10.5246/jcps.2014.12.110

中国药学(英文版) ›› 2014, Vol. 23 ›› Issue (12): 866-872.DOI: 10.5246/jcps.2014.12.110

RP-HPLC-DAD法同时测定毛冬青根中4种三萜皂苷和2种木脂素的含量

周渊¹, 李宁¹, 张加余², 姜勇¹, 屠鹏飞^1,3*

1. 北京大学医学部药学院天然药物及仿生药物国家重点实验室, 北京 100191
2. 北京中医药大学科研实验中心, 北京 100029
3. 北京中医药大学中医药现代研究中心, 北京 100029

收稿日期:2014-08-20 修回日期:2014-09-24 出版日期:2014-12-25 发布日期:2014-10-11
通讯作者: Tel./Fax: 86-10-82802750
基金资助:
Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20110001130003); the National Key Technology R&D Program “New Drug Innovation” of China (Grant No. 2012ZX09301002-002-002 and 2012ZX09304-005).

Simultaneous determination of four triterpenoid saponins and two liganoids in the roots of Ilex pubescens by RP-HPLC-DAD

Yuan Zhou¹, Ning Li¹, Jiayu Zhang², Yong Jiang¹, Pengfei Tu^1,3*

1. State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100191, China
2. Center of Scientific Experiment, Beijing University of Chinese Medicine, Beijing 100029, China
3. Modern Research Center for Traditional Chinese Medicine, Beijing University of Chinese Medicine, Beijing 100029, China

Received:2014-08-20 Revised:2014-09-24 Online:2014-12-25 Published:2014-10-11
Contact: Tel./Fax: 86-10-82802750
Supported by:
Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20110001130003); the National Key Technology R&D Program “New Drug Innovation” of China (Grant No. 2012ZX09301002-002-002 and 2012ZX09304-005).

摘要/Abstract

摘要：

建立了反相高效液相色谱-二极管阵列检测法同时测定毛冬青根中的6种活性成分 (tortoside A, (+)-丁香脂素, 毛冬青皂苷B₃, 毛冬青皂苷A₁, 毛冬青皂苷B₁, 毛冬青素A) 的含量。RP-HPLC分离用反相C₁₈分析柱, 流动相以乙腈-0.1%磷酸水体系梯度洗脱。流速1.0 mL/min, 检测波长为210 nm。6个指标成分达到基线分离, 标准曲线具有良好的线性 (r²>0.9996), 精密度、稳定性和重复性符合分析方法学要求。加样回收率范围为99.00%-104.52%。最后对15个批次的毛冬青药材含量测定结果进行了聚类分析。结果表明该方法不仅可以对毛冬青药材进行质量控制, 而且也为毛冬青药材的道地性分析提供了科学依据。

关键词: 高效液相色谱, 冬青属, 毛冬青, 三萜皂苷, 木脂素, 聚类分析

Abstract:

A reversed-phase high performance liquid chromatography (RP-HPLC) method with diode array detector (DAD) has been established to simultaneously determine six bioactive compounds in the roots of Ilex pubescens, namely tortoside A, (+)-syringaresinol, ilexsaponin B₃, ilexsaponin A₁, ilexsaponin B₁, ilexgenin A. The RP-HPLC assay was performed on a reversed-phase C₁₈ column with a gradient elution. The mobile phase consisted of acetonitrile and water containing 0.1% (v/v) phosphoric acid. The flow rate was 1.0 mL/min and the detection wavelength was set at 210 nm. The six marker constituents were separated well with good linearity (r²>0.9996), precision, stability and repeatability. The overall recoveries were in the range of 99.00%–104.52%. Cluster analysis was employed to analyze 15 batches of samples. The result indicated this method provide an efficient way to perform quality control as well as a scientific rationale for the Geo-authentication of I. pubescens.

Key words: RP-HPLC-DAD, Aquifoliaceae, Ilex pubescens, Triterpenoid saponin, Liganoid, Cluster analysis

中图分类号:

R284

Supporting:

周渊, 李宁, 张加余, 姜勇, 屠鹏飞. RP-HPLC-DAD法同时测定毛冬青根中4种三萜皂苷和2种木脂素的含量[J]. 中国药学(英文版), 2014, 23(12): 866-872.

Yuan Zhou, Ning Li, Jiayu Zhang, Yong Jiang, Pengfei Tu. Simultaneous determination of four triterpenoid saponins and two liganoids in the roots of Ilex pubescens by RP-HPLC-DAD[J]. Journal of Chinese Pharmaceutical Sciences, 2014, 23(12): 866-872.

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RP-HPLC-DAD法同时测定毛冬青根中4种三萜皂苷和2种木脂素的含量

Simultaneous determination of four triterpenoid saponins and two liganoids in the roots of Ilex pubescens by RP-HPLC-DAD

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