普那霉素ⅠA纯化工艺研究  

Studies on the purification technology of pristinamycin ⅠA

作　　者：李晓露[1] 高月麒 王海燕[1] 林旸[1] 王宁[1] 任风芝[1] 张雪霞[1] 

机构地区：[1]微生物药物国家工程研究中心,河北省工业微生物代谢工程技术研究中心,华北制药集团新药研究开发有限责任公司,石家庄050015

出　　处：《中国抗生素杂志》2017年第9期771-774,共4页Chinese Journal of Antibiotics

基　　金：国家“重大新药创制”科技专项(No.2014ZX09201001)

摘　　要：目的开发一种普那霉素ⅠA纯化工艺。方法使用中压层析系统,以普那霉素ⅠA收率为指标,考察反相硅胶C18的洗脱参数和上样量,并对结晶条件进行优选。结果 30μm的反相硅胶C18为最佳层析介质,洗脱剂为体积分数55%的甲醇-酸水溶液,流速为1.5BV/h层析柱体积,上样量为10mg/m L层析介质;结晶溶剂为乙酸乙酯,结晶浓度为100~120mg/m L;按此工艺所得产品纯度大于98.5%,总收率大于70%。结论此种普那霉素ⅠA的纯化方法简单易行,收率稳定,为其规模化生产提供了参考。Objective To develop a purification process for pristinamycin I A. Methods Using the medium pressure chromatography system, elution parameters and loading capacity were investigated on reversed-phase silica gel C 18. The purification efficiency was evaluated by the yield of pristinamycin I A. The crystallization condition was optimized at the same time. Results Reversed-phase silica gel C 18 with a diameter of 30pm was selected as the best chromatography medium. The optimal conditions are described as follows： 55% methanol-H20 was used as the eluant with the flow rate of 1.5BV/h and the loading amount of sample was 10mg/mL in the medium. Ethyl acetate was used as the crystallization solvent, and the crystallization concentration was 100-120mg/mL. The purity of the final product was more than 98.5% and the yield of pristinamycin I A was above 70% under the optimal conditions. Conclusion The purification method is simple and stable, and provides a reference for the large-scale preparation of pristinamycin I A.

关 键 词：普那霉素 反相硅胶 分离纯化 

分 类 号：R978.1[医药卫生—药品]