摘要
用硫酸溶液从黄藤中提取巴马汀,用大孔树脂富集,使用正交试验优选出还原巴马汀制备延胡索乙素的工艺。在还原的正交试验中,还原剂和催化剂用量是影响产率的主要因素。巴马汀还原条件(乙醇浓度为80%、还原剂∶巴马汀=3∶1、催化剂∶巴马汀=1.5∶1)下制备延胡索乙素,粗产率可达88%~90%。碱性氧化铝分离后,产物与延胡索乙素对照品的PLC、熔点、紫外光谱的测定结果以及产物的核磁共振波谱结果表明,所得产物为延胡索乙素。
Palmatine was extracted from Caulisfibraureae with sulfuric acid solution, and then concentrated by macroporous resin. Orthogonal Optimization was used to optimizate the reduction process of the palmatine to make tetrahydropalmatine. In the orthogonal experiment, the amount of reducing agent and the amotmt of catalyst were the main factors affected the yield. Tetrahydropalmatine was prepared with reducing palmatine and the crude yield was up to 90% under these conditions: ethanol concentration 80%, reductant:palmati ne=3 : 1,catalyst: palmatine=l.5 : 1. Crude tetrahydropalmatine was separated with basic alumina. The determination of TLC, melting point, UV spectroscopy of the sample and the control sample, and nuclear magnetic resonance spectroscopy of the sample results showed that the product was tetrahydropalmatine.
出处
《化工技术与开发》
CAS
2015年第6期8-10,15,共4页
Technology & Development of Chemical Industry
基金
广东省教育部产学研项目(2011B090400416)
中山市科技计划项目(20123A317)
关键词
黄藤
巴马汀
延胡索乙素
还原
Caulisfibraureae
palmatine
tetrahydropalmatine
reduction