摘要
采用连续中压硅胶柱色谱法纯化紫杉醇。优化的工艺条件为:以中压玻璃柱为色谱柱,120～160μm层析硅胶为填料,1%紫杉醇负载量为2g/100g硅胶,样品二氯甲烷溶解上样,二氯甲烷:乙腈(7:3)洗脱,洗脱流速为60mL/min。一次柱色谱过程即可得到纯度大于90%紫杉醇,回收率75%以上,甲醇:水3:1(v/v)重结晶后得纯度99%紫杉醇产品,低纯度组分作为层析原料再次纯化。使用后的层析柱用二氯甲烷:乙腈(1:1)再生,二氯甲烷平衡,平衡后的层析柱重复使用,使用5次柱分离效率仍不降低。与传统方法相比溶剂用量少、层析填料价格低、生产周期短、分离效果好,易于实现连续工业化清洁生产。
A method is described for successive purification of paclitaxel by medium - pressure silica gel column chroma- tography. The optimuru condition was as foUowed ：The chromatographic column was moderatepressure glass column, 120 -160 μm silica gel as filling material, 1% paclitaxel loading amount 2g/100g silica gel, the samples was dissolved in dichloron.romethane, the mobile phase were dichloromethane： acetonitrile （7：3）, the flow rate was 60mL/min, the receive ratio of the paclitaxel was over 75% through one silica gel chromatographic column, and the pretty of paclitaxel was 99% after crystallization with methanol：water（ 3：1 ）, the low purity compounds were purification again. The used chromatographic column was regeneration with dichloromethane ： acetonitrile （ 1：1 ）, then equilibrium with dichloromethane, the regeneration chromatographic column can be reusable, and the efficiency for separation were nearly no depressed ,＇ffter used five times. In comparison to the traditional methods, the method has its own characteristics with low solvent consumption; low price of chromatograph fillers, short cycle time, separating effect is better,easy to realize industrialization cleaner production.
出处
《黑龙江医药》
CAS
2013年第1期28-31,共4页
Heilongjiang Medicine journal
基金
公益性行业科研专项(201204601)资助
关键词
紫杉醇
柱色谱
纯化
paclitaxel
colunm chromatography
purification
