摘要
目的 开发一种他克莫司的分离提纯工艺。方法 采用离子交换树脂脱色除杂、纳滤、结晶等手段得到高质量的他克莫司粗粉,再经反相色谱硅胶层析、复合溶液结晶,得到符合USP标准的他克莫司精粉。结果 优选的脱色树脂为D002,所得他克莫司粗粉效价大于800μg/mg,二氢他克莫司含量小于4%;该粗粉经UniSil C8Ultra Plus层析纯化,精粉含量大于99.5%,最大单杂小于0.1%。结论 该工艺操作简单、能耗低、收率高,适于他克莫司的产业化应用。
Objective The purpose of this study is to develop a separation and purification process for tacrolimus.Methods Tacrolimus coarse powder with high purity was obtained by ion exchange resin decolorization,nanofiltration and crystallization,which was further refined by reverse phase chromatography silica gel chromatography and composite solution crystallization to obtain the tacrolimus product that can meet USP standards.Results The optimized decolorizing resin was D002.The titer of the tacrolimus coarse powder was more than 800μg/mg and the purity of the dihydro-tacrolimus was less than 4%.Then we continued to purify the coarse powder using UniSil C8 Ultra Plus chromatography to obtain the fine powder.And the purity of the tacrolimus fine powder was more than 99.5%;the maximum single impurity substance was less than 0.1%.Conclusion This method had the characteristics of simple operation,low energy consumption and high yield,which were of great significance to the industrial production of tacrolimus.
作者
王圆超
赵辉
王月
谷岩翡
高月麒
李晓露
Wang Yuanchao;Zhao Hui;Wang Yue;Gu Yanfei;Gao Yueqi;Li Xiaolu(National Engineering Research Center of Microbial Medicine,Shijiazhuang Microbial Drug Technology Innovation Center,New Drug Research&Development Company of NCPC,Shijiazhuang 052165;Huasheng Company of NCPC,Shijiazhuang 052160)
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2024年第2期175-180,共6页
Chinese Journal of Antibiotics
基金
河北省科技研发平台建设专项(No.22567651H)
石家庄市技术创新中心绩效后补助(No.237790659A)。
关键词
他克莫司
分离提纯
离子交换树脂
层析
结晶
Tacrolimus
Separation and purification
Ion exchange resin
Chromatography
Crystallization
