紫杉烷二萜类化合物10-DABⅢ的分离纯化

Study on Separation and Purification of Taxane Diterpenoids Compound 10-DABⅢ

目的:建立分离纯化紫杉烷二萜类化合物10-脱乙酰基巴卡亭Ⅲ(10-DABⅢ)的方法。方法:采用柱层析和重结晶的方法精制10-DABⅢ。以杂质含量为指标确定层析液比例;以纯度和收率为指标筛选第1次重结晶时三氯甲烷的用量,第2次重结晶时丙酮、正己烷的用量以及2次重结晶的温度和时间。结果:层析液丙酮与三氯甲烷体积比为2.25:7.75,此时杂质含量最小,为3.7%。用15倍体积(W/V)的三氯甲烷、-25℃冷冻24h第1次重结晶以及35倍体积的丙酮(W/V)和30倍体积的正己烷(W/V)、-25℃冷冻12h第2次重结晶,纯化后的样品纯度为99.34%,收率为83.50%。结论:该方法对10-DABⅢ分离纯化效果好。

OBJECTIVE： To establish the method for the separation and purification of taxane diterpenoids compound 10-deacetylbaccatin Ⅲ （10-DABⅢ ）. METHODS： 10-DAB Ⅲ was refined by using column chromatography and recrystallization, and the proportion of chromatography liquid was determined using the content of impurity; the amount of chloroform was selected at the first recrystallization, the amounts of acetone and n-hexane at the second recrystallization and the temperature and time of re- crystallization were selected using purity and yield as index. RESULTS： The optimal technology was as follows： ratio of acetone to chloroform was 2.25：7.75, the content of impurity was the least （3.7%）. 15 times the volume of chloroform （W/V） was frozen at --25 ℃ for 24 h at the first recrystallization; 35 times the volume of acetone （W/V） and 30 times the volume of hexane （W/V） were frozen at --25 ℃ for 12 h at the second recrystallization. The purity of sample was 99.34% after purification and the yield of samples was 83.50%. CONCLUSION： The technology has good purification for the refinement of 10-DABⅢ.