天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (5): 716-720.

• 研究简报 • 上一篇    下一篇

UPLC-QTof-MS测定不同提取条件下柴胡皂苷a和柴胡皂苷d的转化规律

郭 智1,彭 冰2,李宗阳1,潘瑞乐1*   

  1. 1 中国医学科学院北京协和医学院药用植物研究所,北京 100193;2 首都医科大学附属北京中医医院 北京 100010 
  • 出版日期:2014-05-31 发布日期:2014-11-17

Study on Transformation Rule of Saikosaponin a and Saikosaponin d Under Different Extraction Conditions by UPLC-QTof-MS

GUO Zhi1, PENG Bing2, LI Zhong-yang1, PAN Rui-le1*   

  1. 1 Institute of Medicinal Plant development,Chinese Academy of Medical Sciences and Peking Union Medical College, Beijing 100193,China;  2 Beijing Hospital of TCM Affiliated to Capital University of Medical Science,Beijing 100010,China
  • Online:2014-05-31 Published:2014-11-17

摘要: 使用UPLC-QTof-MS研究了不同提取条件下柴胡皂苷a、d的转化规律。色谱柱为Acquity UPLC BEH C18(2.1 mm×50 mm,1.7 μm);流动相为乙腈-0.01%甲酸水溶液;流速为0.45 mL/min。以四极杆串联飞行时间质谱(Q-Tof)为检测器,使用负离子检测模式,对经过12种不同提取方法提取的柴胡样品(1~12)进行检测。得到柴胡皂苷a、d不同提取方法下的转化规律:酸性常温条件下水解生成柴胡皂苷b1、b2,酸性加热情况下糖苷键水解生成皂苷元;中性、碱性条件下均较稳定。实验结果对柴胡皂苷a、d的提取、分离、分析提供了参考依据。

关键词: UPLC-QTof-MS, 柴胡皂苷a, 柴胡皂苷d, 柴胡皂苷b1, 柴胡皂苷b2, 提取

Abstract: The transformation rules of saikosaponin a and saikosaponin d under different extraction methods were studied by ultra-performance liquid chromatography coupled with Quadrupole-time of flight mass spectrometry (UPLC-QTof-MS).A new UPLC-QTof-MS method was developed for profiling and quantification of the transformation products of saikosaponin a and saikosaponin d under different extraction methods.Chromatographic separation was performed on an Acquity UPLC BEH C18 column (2.1 mm×50 mm,1.7 μm) with a mobile phase consisting of acetonitrile (A) and 0.01% formic acid in water (B).The flow rate was kept constant at 0.45 mL/min with a gradient elution.QTof-MS was used as the detector.Twelve samples of Radix Bupleuri were individually extracted using 12 different extraction methods and were then analyzed by UPLC-QTof-MS with negative ion mode.The transformation rule of saikosaponin a and saikosaponin d under different extraction methods were derived:saikosaponin a and saikosaponin d were hydrolyzed into saikosaponin b1 and saikosaponin b2 under acidic condition at at room temperature.The glycosidic bond was hydrolyzed yielded to sapogenin under acid condition and being heated.Saikosaponin a and saikosaponin d were stable under neutral and alkaline condition.The experimental results provided a refrence for extraction,separation and analysis of saikosaponin a and saikosaponin d.

Key words: UPLC-QTof-MS, saikosaponin a, saikosaponin d, saikosaponin b1, saikosaponin b2, extraction

中图分类号: 

R932