新药五味子乙素中主要相关物质的分离和结构鉴定

Separation and Structure Identification of the Primary Impurity in γ-Schizandrin

目的对创新药物五味子乙素中主要相关物质进行分离和结构鉴定。方法采用柱层析及制备HPLC方法从五味子乙素结晶母液中分离得到成品原料的一个主要微量化学成分,通过NMR、MS、CD等波谱方法鉴定化合物结构,运用HPLC-UV方法进行质量分数检测。结果制备分离得到的未知杂质为Isokadsuranin,质量分数>98%。结论本法得到的Isokadsuranin符合中药化学对照品的相关技术要求,为创新药物五味子乙素的质量控制研究提供化学对照品。

Objective To separate and identify the primary impurity from a new drug, ？-Schizandrin. Methods Column chromatography and preparative HPLC were used to separate the major impurity from the bulk drug of γ-Schizandrin. Its structure was characterized by NMR, MS, and CD spectroscopic analysis, and the purity was detected by HPLC-UV. Results The unknown impurity was identified as Isokadsuranin, and the purity of the reference substance was more than 98 %. Conclusion The related substance ofisokadsuranin acquired by this method could meet the requirements of related chemical reference substance in Chinese materia medica. It could be used as a chemical reference substance for quality control of the new drug, γ-Schizandrin.