石杉碱甲的分离纯化工艺

Study on the separation and purification technics of huperzine A

目的:研究一种石杉碱甲的工业化分离纯化工艺,以达到批量生产之目的。方法:通过对石杉碱甲理化性质的分析,以中性氧化铝为填料对石杉碱甲粗品进行柱色谱分离纯化,采用薄层色谱-柱色谱考察了各因素的影响,以石杉碱甲回收率和含量为考察指标,寻找最佳工艺参数。结果:柱色谱最佳分离条件为:洗脱剂体系为氯仿-甲醇(v/v)=100∶5,100∶10,流速为3mL.min-1,柱床体积比为25∶1,进料量为10 mL,柱温为室温,在此条件下石杉碱甲回收率达97.6%,含量达99.2%。结论:该工艺条件能够在简单的条件下实现石杉碱甲批量分离纯化,具有工业应用价值。

OBJECTIVE To study the separation and purification process of huperzine A for industrialization, and to achieve mass production purposes. METHODS Through analysis of the physical and chemical properties of huperzine A , a neutral aiumina was found as filler for purification of huperzine A crude product by column chromatography; thin-layer chromatography column chromatogram was adopted for study of the impact of various factors; the content and recovery of huperzine A were taken as the indexes to find the best process parameters. RESULTS The best separation conditions for column chromatogra phy： eluent system chloroform： methanol （v/v） = 100： 5,100： 10, flow rate 3 mL.min -1 , column bed volume ratio of 25 ： 1, feed volume of 10 mL, the column temperature was at room temperature, in this condition huperzine A recovery rate was 97.6%, content concentration of 99. 2%. CONCLUSION The process conditions in the most simple conditions can achieve huperzine A batch purified with strong industrial applications.