环孢素衍生物(γ-hydroxylmethylleucine4)-cyclosporin A的分离纯化与鉴定

摘要

目的 研究高纯度环孢素衍生物(γ-hydroxylmethylleucine4)-cyclosporin A的分离纯化工艺.方法 采用HPLC检测方法,以大孔树脂、聚合物微球为载体进行分离纯化.利用质谱(Ms)和核磁共振谱(NMR)解析化合物的结构.结果 发酵液经过滤,吸附,结晶得到粗提物,粗提物再经聚合物微球,浓缩,萃取,结晶得到高纯度产品,光谱数据确定为(γ-hydroxylmethylleucine4)-cyclosporin A,所得产品纯度≥95％,收率大于70％.结论 建立(γ-hydroxylmethylleucine4)-cvclosporinA的分离纯化工艺,流程简单、可行,为该产品产业化开发提供基础.%Objective To study the separation and purification process of high-purity (γ-hydroxyl-methylleucine4)-cyclosporin A.Methods (γ-hydroxylmethylleucine4)-cyclosporin A was separated and purified by macroporous resin and nanoscale polymer particles.The chemical structure was analyzed by the spectral analysis including MS and NMR.Results The crude (γ-hydroxylmethylleucine4)-cyclosporin A was obtained from the fermentation broth by methods of filtration,adsorption and crystallization.After a further purification by nanoscale polymer particles,concentration,solvent extraction and crystallization,the high purity (γ-hydroxylmethylleucine4)-eyclosporin A was isolated.The structure was identified by spectral data.The purity of the final product was more than 95％ and the total yield was above 70％.Conclusion The established purification process was simple and feasible for further industrialization of this product.