【摘要】 为了确定环孢菌素A结晶工艺,对溶剂种类、反溶剂加入量、结晶温度和降温方式等因素的影响进行研究。首先通过静态结晶研究,确定了丙酮/水结晶体系和溶剂比例。在此基础上,设计了正交试验L9(34)考察动态结晶中各因素对环孢菌素A结晶收率和纯度的影响,并进一步优化了结晶降温方式。结果表明:确定环孢菌素A结晶的最佳条件为采用梯度程序降温,养晶温度为-5℃,丙酮和水的体积比为2∶1,反溶剂水流加时间为0.5 h,开始流加点为降温至0℃,结晶时间约为3 h。经HPLC分析环孢菌素A的纯度平均值为99.15%,收率平均值为87.7%。更多还原

【Abstract】 The crystalization technology of cyclosporine A was studied by using single factor test and orthogonal experiment design.Effects of different solvents,solvent ratio,and temperature on the crystallization were investigated.Results revealed that the water content had important effects on the purity and recovery of cyclosporine A and crystallization temperature was also another important factor.The optimum crystalization conditions of cyclosporine A were determined as follows: the cooling in gradient was applied;crystal temperature was-5 ℃;solvent ration was 2∶1(acetone∶water),feeding time of water was 30 min;and crystallization period was 3 h.The average HPLC purity of cyclosporine A reached 99.15%.The average crystalline recovery was 87.7%.更多还原