常压柱色谱组合法制备石杉碱甲  

Preparation of huperzine A by manufacturing technique of assembling column chromatograph at normal pressure

作　　者：徐朝晖[1] 郑向炜[1] 高君伟[1] 阮克锋[1] 冯怡[1] 

机构地区：[1]上海中医药大学中药现代制剂技术教育部工程研究中心,上海201203

出　　处：《中国新药与临床杂志》2012年第12期732-736,共5页Chinese Journal of New Drugs and Clinical Remedies

基　　金：上海市教委重点学科资助(J50302)

摘　　要：目的寻求一条经济实用、便于产业化的石杉碱甲制备工艺路线。方法以薄层色谱法选择柱色谱分离系统后,以回收率和含量为考察指标,对影响柱色谱分离效果的各因素进行选择与优化,寻找最佳工艺路线。结果采用碱性氧化铝柱和硅胶柱的组合进行分离纯化,碱性氧化铝柱的工艺参数为:填料粒度100～200目,干法装柱(径高比1:10),干法上样(上样比例1:50),三氯甲烷-甲醇(47:3,V/V)洗脱;硅胶柱的工艺参数为:填料粒度200～300目,湿法装柱(径高比1:10),湿法上样(上样比例1:30),三氯甲烷-甲醇(48:2,V/V)洗脱。所得产物溶于丙酮,静置过夜后,即可获得符合《中国药典》要求的结晶产物,本工艺条件下的石杉碱甲总回收率达到76.1%。结论本工艺设备要求简单,样品处理量大,生产成本低,适合工业化生产。AIM To explore an economical and practical scale preparation technique for huperzine A. METHODS The chromatographic solvent system was selected by thin layer chromatography, and various optimal factors were studied based on the content and recovery of huperzine A. RESULTS Normal-pressure column chromatography on alumina B and silica gel were used to isolate and purify huperzine A. The parameters of column chromatograph on alumina B： the size of alumina B is 100 - 200, dry column-packing （diameter via height ratio 1 ： 10）, dry sample loading （loading ratio 1 ： 50）, eluted with chloroform-methanol （47 ： 3, V/V）. The parameters of column chromatograph on silica gel： the size of silica gel is 200 - 300, wet columnpacking （diameter via height ratio 1 ： 10）, wet sample loading （loading ratio 1 ： 30）, methanol （48 ： 2, V/V）. The fraction was dissolved in acetone overnight at 4 ℃ eluted with chloroform, and then crystallinehuperzine A huperzine A suits to scale was obtained which could meet the is 76.1%. CONCLUSION This simple manufacture standard of Chinese Pharmacopoeia. The total recovery of technology could deal with large samples economically and

关 键 词：石杉碱甲 阿尔茨海默病 色谱法 薄层 氧化铝 常压柱层析 硅胶 

分 类 号：R931[医药卫生—生药学] R971[医药卫生—药学]