HPLC/DAD/ESI-MSn方法鉴定开心散的化学成分及其体内代谢产物

doi:10.5246/jcps.2012.06.072

HPLC/DAD/ESI-MSn方法鉴定开心散的化学成分及其体内代谢产物

刘春芳, 杨文志, 刘珂弟, 乔雪, 刘洋, 姜艳艳, 石任兵^*, 薄涛, 杨秀伟, 叶敏^*

1. 北京大学医学部天然药物及仿生药物国家重点实验室; 药学院, 北京 100191
2. 北京中医药大学中药学院, 北京 100102
3. 安捷伦科技有限公司, 北京 100102

收稿日期:2012-06-04 修回日期:2012-08-15 出版日期:2012-10-25 发布日期:2012-10-25
通讯作者: 石任兵*, 叶敏*

Characterization of chemical constituents and in vivo metabolites of Kai-Xin-San prescription by HPLC/DAD/ESI-MSn

Chunfang Liu, Wenzhi Yang, Kedi Liu, Xue Qiao, Yang Liu, Yanyan Jiang, Renbing Shi*, Tao Bo, Xiuwei Yang, Min Ye^*

1. State Key Laboratory of Natural and Biomimetic Drugs, School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100191, China
2. School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100102, China
3. Agilent Technologies, Inc., 3 North Wangjing Road, Beijing 100102, China

Received:2012-06-04 Revised:2012-08-15 Online:2012-10-25 Published:2012-10-25
Contact: Renbing Shi*, Min Ye*

摘要/Abstract

摘要：

为了研究开心散的化学成分及体内代谢产物, 采用Agilent SB-C₁₈色谱柱, 利用离子阱质谱及高分辨飞行质谱对开心散提取物及口服开心散后的大鼠血浆样品进行分析。从开心散提取物中共鉴定了39个化学成分, 包括11个人参皂苷, 14个远志皂苷, 5个远志多糖, 8个远志寡糖酯及1个远志口山酮, 其中15个化合物通过与对照品对照确定, 未检测到茯苓及石菖蒲的成分。大鼠灌胃给予开心散提取物后 (7 g/kg), 从血浆检测到10个人参皂苷和18个远志成分。本研究表明, 人参皂苷、远志皂苷及糖酯很可能是开心散的主要有效成分。

关键词: 开心散, 化学分析, 代谢产物鉴定, HPLC/DAD/ESI-MSn

Abstract:

This work aims to elucidate the chemical constituents of Kai-Xin-San (KXS) and its metabolites in rat plasma. KXS extracts were separated on an Agilent HPLC SB-C₁₈ column, analyzed by ion-trap tandem mass spectrometry and high-accuracy qTOF mass spectrometry in negative ion mode. A total of 39 compounds, including 11 ginsenosides, 14 Polygala saponins, 5 sucrose esters, 8 oligosaccharide esters and 1 xanthone were characterized from KXS. Fifteen of them were confirmed by reference standards. No constituents were detected from Poria or Acori Tatarinowii Rhizoma. After oral administration of KXS (7 g/kg), 10 ginsenosides and 18 Polygala compounds were detected in rat plasma. This study indicates that ginseng saponins, Polygala saponins and saccharide esters could be the major effective components of KXS prescription.

Key words: Kai-Xin-San, Chemical analysis, Metabolites identification, HPLC/DAD/ESI-MSn

中图分类号:

R931

Supporting:

Foundation items: National Science & Technology Mega Project for Primary Drug Innovation from Ministry of Science and Technology of China (Grant No. 2009ZX09502-006).
^*Corresponding author. Tel./Fax: 86-10-82801516;
E-mail: yemin@bjmu.edu.cn; shirb@126.com
Dedicated to Professor Lihe Zhang on the occasion of his 75^th birthday.

刘春芳, 杨文志, 刘珂弟, 乔雪, 刘洋, 姜艳艳, 石任兵^*, 薄涛, 杨秀伟, 叶敏^*. HPLC/DAD/ESI-MSn方法鉴定开心散的化学成分及其体内代谢产物[J]. , DOI: 10.5246/jcps.2012.06.072.

Chunfang Liu, Wenzhi Yang, Kedi Liu, Xue Qiao, Yang Liu, Yanyan Jiang, Renbing Shi*, Tao Bo, Xiuwei Yang, Min Ye^*. Characterization of chemical constituents and in vivo metabolites of Kai-Xin-San prescription by HPLC/DAD/ESI-MSn [J]. , DOI: 10.5246/jcps.2012.06.072.

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