天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (3): 427-430.

• 开发研究 • 上一篇    下一篇

微波辐射合成小檗红碱的工艺研究

刘丽贤1,2, 袁晓2, 高英3, 周东斌2, 李卫民1*   

  1. 1 广州中医药大学中药学院,广州 510006;2 广州牌牌生物科技有限公司,广州 510000;3 广州中医药大学新药中心,广州 510006
  • 出版日期:2014-03-29 发布日期:2014-12-08

Synthesis of Berberrubine under Microwave Irradiation

LIU Li-xian1,2, YUAN Xiao2, GAO Ying3, ZHOU Dong-bin2, LI Wei-min1*   

  1. 1 College of Chinese Materia Medica,Guangzhou University of Chinese Medicine,Guangzhou 510006,China;2 PI & PI Biotechnology (Guangzhou) INC,Guangzhou 510000,China;3 New Drug R&D Center, Guangzhou University of Chinese Medicine,Guangzhou 510006,China
  • Online:2014-03-29 Published:2014-12-08

摘要: 首次以DMF为反应介质,微波法快速合成小檗红碱。通过单因素法,考察了反应功率、液料比、反应时间对产率的影响,并采用析晶的方法纯化产物,产品纯度和结构经HPLC、UV、IR、ESI-MS、1H-NMR、13C-NMR确定,得出最佳合成工艺条件:微波功率400 W、微波时间15 min、小檗碱与DMF料液比为1:25(g:mL),析晶纯化,纯度98%,收率93%。并与传统的真空热解法相比,微波辅助合成可使产率提高近15%,反应时间缩短近4倍;且反应物纯度高(≥95%),可直接析晶纯化,方法经济简便。

关键词: 小檗红碱, 微波, 合成, 小檗碱, 真空热解

Abstract: In this study,DMF was adopted as reaction medium for the first time in the synthesis of berberrubine under microwave irradiation.The effect of reaction power,solid-liquid ratio and reaction time on yield of berberrubine was studied using single factor tests.After crystallization and purification,the purity and structure of berberrubine was tested by HPLC,UV,IR,ESI-MS,1H-NMR and 13C-NMR.The optimal synthetic conditions were determined to be:microwave power 400 W, microwave time 15 min,berberine/DMF ratio 1:25 (g:mL).The yield was up to 93% under the optimized experimental conditions and the purity of berberrubine after purification was as high as 98%.Compared with traditional method of synthesizing berberrubine by vacuum pyrolysis,the yield of berberrubine under microwave irradiation was increased by nearly 15% while the reaction time was shortened by 4 times.In addition,the purification process was economic and simple.

Key words: berberrubine, microwave, synthesis, berberine, vacuum pyrolysis

中图分类号: 

O629.3 R284.3