色谱

色谱 ›› 2011, Vol. 29 ›› Issue (05): 430-434.DOI: 10.3724/SP.J.1123.2011.00430

• 研究论文 • 上一篇    下一篇

生附子中C19型二萜生物碱的高速逆流色谱分离及其结构鉴定

刘敏卓1, 张思佳1, 杨春华2, 夏烨1, 刘静涵1, 梁敬钰1*   

  1. 1. 中国药科大学天然药物化学教研室, 江苏 南京 210009; 2. 中国药科大学分析测试中心, 江苏 南京 210009
  • 收稿日期:2011-01-05 修回日期:2011-03-03 出版日期:2011-05-28 发布日期:2011-05-28
  • 通讯作者: 梁敬钰,教授. Tel: (025)83271406
  • 基金资助:
    中国药科大学研究生基本科研业务费专项资金项目(No. 02410088).

high-speed counter-current chromatography (HSCCC)| diterpenoid alkaloids| beiwutine| mesaconitine| hypaconitine| Aconitum carmichaeli

LIU Minzhuo1, ZHANG Sijia1, YANG Chunhua2, XIA Ye1, LIU Jinghan1, LIANG Jingyu1*   

  1. 1. Department of Phytochemistry, China Pharmaceutical University, Nanjing 210009, China; 2. Center for Instrumental Analysis, China Pharmaceutical University, Nanjing 210009, China
  • Received:2011-01-05 Revised:2011-03-03 Online:2011-05-28 Published:2011-05-28

PDF

559

被引次数

24

摘要： 应用高速逆流色谱法分离制备了生附子中的3个C19型二萜生物碱类化合物。以正己烷-乙酸乙酯-甲醇-水(3:5:4:5, v/v/v/v)为两相溶剂系统,上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2.0 mL/min、检测波长235 nm条件下进行分离制备;一次性从90 mg附子总碱粗提物中分离制备得到15.3 mg北草乌碱,35.1 mg中乌头碱和22.7 mg次乌头碱,经高效液相色谱分析,测得它们的纯度分别为97.9%、96.2%和99.2%。并应用波谱(电喷雾离子质谱、核磁共振氢谱和核磁共振13C谱)解析法确定了它们的结构。利用该方法可以对生附子中的二萜类生物碱成分进行快速的分离和纯化

关键词: 北草乌碱, 次乌头碱, 二萜生物碱, 高速逆流色谱法, 生附子, 中乌头碱

Abstract: Abstract: A new method for preparative isolation and purification of C19 diterpenoid alkaloids beiwutine, mesaconitine and hypaconitine from the lateral roots of Aconitum carmichaeli Debx. (Fuzi in Chinese) by high-speed countercurrent chromatography was established. n-hexane-ethyl acetate-methanol-water (3 : 5 : 4 : 5, v/v/v/v) was used as the two phase solvent system.15.3mg of beiwutine,35.1mg of mesaconitine and 22.7 mg of hypaconitine were obtained from 90 mg of crude extracts in one-step separation. The structures of these three compounds were identified by ESI-MS, 1H-NMR and 13C-NMR.The purity of beiwutine, mesaconitine and hypaconitine was 97.9%,96.2% and 99.2%, respectively, as determined by high performance liquid chromatography (HPLC).

Key words: Aconitum carmichaeli, Beiwutine, Diterpenoid alkaloid, Hypaconitine, Mesaconitine, Keywords HSCCC