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林产化学与工业 ›› 2015, Vol. 35 ›› Issue (2): 86-90.doi: 10.3969/j.issn.0253-2417.2015.02.013

• 研究报告 • 上一篇    下一篇

高速逆流色谱法分离制备太白贝母中贝母辛

姜艳1, 戴静1, 萧伟2, 赵林果1   

  1. 1. 南京林业大学 化学工程学院, 江苏 南京 210037;
    2. 江苏康缘药业股份有限公司, 江苏 连云港 222001
  • 收稿日期:2014-09-17 出版日期:2015-04-25 发布日期:2015-04-24
  • 通讯作者: 萧伟,教授,博士生导师,主要从事中药新品种、新工艺和新剂型的开发与研究;E-mail:xw@kanion.com。 E-mail:xw@kanion.com
  • 作者简介:姜艳(1977-),女,江苏泰兴人,副教授,博士,主要从事天然活性成分研究;E-mail:jiangyancpu@126.com
  • 基金资助:
    江苏省自然科学基金资助项目(BK2012419);国家自然科学基金资助项目(31400300)

Isolation and Purification of Peimisine from Fritillaria taipaiensis Bulbs by High-speed Counter-current Chromatography

JIANG Yan1, DAI Jing1, XIAO Wei2, ZHAO Lin-guo1   

  1. 1. College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037, China;
    2. Jiangsu Kanion Pharmaceutical Co., Ltd., Lianyungang 222001, China
  • Received:2014-09-17 Online:2015-04-25 Published:2015-04-24

摘要: 运用高速逆流色谱(HSCCC)技术从太白贝母中分离制备贝母辛。以正己烷/乙酸乙酯/甲醇/水(体积比4:5:3:5)为溶剂体系,转速800 r/min, 流速2.0 mL/min,温度35 ℃,检测波长为215 nm,从50 mg太白贝母总生物碱中经一次HSCCC分离可得到5.3 mg贝母辛,纯度为96.3%,回收率为87.2%。并利用高效液相色谱-四极杆飞行时间质谱(HPLC-QTOF MS)对贝母辛进行了结构确证。

关键词: 高速逆流色谱, 太白贝母, 贝母辛, 分离制备

Abstract: Peimisine, an isosteroidal alkaloid occurring in Fritillaria species, is a semi-synthetic precursor of cyclopamine. In this paper, high-speed counter-current chromatography (HSCCC) was applied to the separation and purification of peimisine from Fritillaria taipaiensis bulbs. The separation was performed on a TBE-300B HSCCC machine, by using solvent system of n-hexane-ethyl and acetate-methanol-water (4:5:3:5, volume ratio) at 35 ℃, rotating speed 800 r/min, flow rate 2.0 mL/min, and detection wavelength 215 nm. After a HSCCC run, 5.3 mg of target compound was obtained from 50 mg of total alkaloid extract, with the purity of 96.3% and the recovery of 87.2%. The structure of the isolate was confirmed by high performance liquid chromatography-quadruple time-of-flight tandem mass spectrometry (HPLC-QTOF MS).

Key words: high-speed counter-current chromatography, Fritillaria taipaiensis, peimisine, isolation and purification

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