大孔树脂法纯化盐酸表柔比星  

Purifi cation of epirubicin hydrochloride by macroporous resin

作　　者：贾淼[1] 裘鹏程[1] 倪国伟[1] 朱津津[1] 谭支敏 汪有贵 张福利[1] 

机构地区：[1]中国医药工业研究总院上海医药工业研究院创新药物与制药工艺国家重点实验室,上海200437 [2]浙江海正药业股份有限公司,台州318000

出　　处：《中国抗生素杂志》2016年第4期271-276,共6页Chinese Journal of Antibiotics

摘　　要：目的研究大孔树脂法分离纯化盐酸表柔比星的工艺条件,以得到高纯度药用级的盐酸表柔比星。方法建立HPLC检测方法,考察树脂对盐酸表柔比星的吸附和解吸性能,以盐酸表柔比星解吸率和纯度为指标,优化上样量和解吸条件等工艺参数。结果筛选出国产NM100型树脂纯化盐酸表柔比星,最大上样量20mg/m L湿树脂,解吸溶剂为12%乙腈的p H4.5盐酸水溶液,收率90%,解吸率96%以上,成品纯度可达99%以上。结论该工艺纯化效果好,收率和解吸率高,适用于高纯度药用级盐酸表柔比星的制备及工业化生产。Objective To study the method that separation and purification of high-purity epirubicin hydrochloride for pharmaceutical use by macroporous resins with high yield and high desorption rate. Methods The methods of pretreatment and regeneration of resins were established. The HPLC method was setup to detect the concentration and the purity of epirubicin hydrochloride. Based on adsorption capacity and elution efficiency of epirubicin hydrochloride, the conditions to separation and purification of epirubicin hydrochloride by macroporous resins were optimized. Results According to experimental datas, a domestic macroporous resin-NM100 was selected as the effective macroporous adsorbent for separation and purification of epirubicin hydrochloride. The maximum loading amount was 20mg/mL, the velocity of dynamic adsorption was 1BV/h, the velocity of dynamic desorption was 4BV/h, the desorption solvent was 12% acetonitrile （ACN） in hydrochloric acid aqueous solution with pH equal to 4.5. Under these conditions, the yield was 90%; the desorption rate was more than 96%; the purity of final product was above 99% at same time. Conclusion This method about separation and purification of high-purity epirubicin hydrochloride for pharmaceutical use was discovered for the first time and was warranted for the commercial process, because it was high yield and high desorption rate.

关 键 词：盐酸表柔比星 大孔吸附树脂 纯化 

分 类 号：R979.1[医药卫生—药品]