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作 者:王海燕[1] 李晓露[1] 高月麒 张丽[1] 任风芝[1] WANG Haiyan LI Xiaolu GAO Yueqi ZHANG Li REN Fengzhi(National Engineering Research Center of Microbial Medicine, Hebei Industry Microbial Metabolic Engineering & Technology Research Center, New Drug Research & Development Company of NCPC, Shijiazhuang 050015)
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,河北石家庄050015
出 处:《中国医药工业杂志》2017年第6期816-820,共5页Chinese Journal of Pharmaceuticals
基 金:国家“重大新药创制”科技专项(2014ZX09201001)
摘 要:采用二元液相分离系统,通过对比柱色谱硅胶、聚合物微球和反相硅胶3种不同类型色谱介质的分离效果和洗脱参数,开发普那霉素ⅡA的制备工艺。结果显示,选用反相硅胶C18为色谱介质,洗脱剂为乙腈∶0.05%磷酸二氢钾溶液(45∶55),上样量0.8 g/100 ml,纯化所得产品纯度≥98.5%,纯化收率≥75%。Using binary high performence liquid phase separation system, the preparation process of pristinamycin IIA was developed by comparing the separation efficiency and elution parameters of three different types of chromatographic media, such as silica gel, polymer microspheres and reversed-phase silica gel. The results showed that the selectivity for pristinamycin IIA was poor on normal phase silica. There was a long tailed peak shown on reversed phase chromatography with polymer microspheres as the media. However, the separation efficiency by reversed-phase medium was excellent under the following conditions: acetonitrile : 0.05% potassium dihydrogen phosphate solution (45 : 55) as the eluent, with the loading amour of 0.8 g sample on every 100 ml chromatographic media, at the flow rate of 6.0 ml/min. The purity of pristinamycin IIA was over 98.5 %, with the yield more than 75 %. This research may provide some references for the development on multiple component drugs.
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