摘要
目的:从西罗莫司片中分离未知杂质,进行结构鉴定和初步生物学活性考察,提高西罗莫司片的质量。方法:采用硅胶柱层析法富集未知杂质粗品,再用制备型高效液相色谱仪进行纯化。应用紫外光谱、红外光谱、质谱、核磁共振谱等波谱分析法对其进行结构鉴定。用二倍稀释法测定其抗真菌活性,用SRB检测其抗肿瘤活性。结果:纯化获得未知杂质的纯度为96.8%,结构鉴定为断雷帕霉素。抗真菌和抗肿瘤活性低于雷帕霉素。结论:断雷帕霉素是西罗莫司片制备中的主要降解杂质,生物学活性低于西罗莫司。
OBJECTIVE:To improve the quality of sirolimus tablets,unknown impurity was isolated from sirolimus tablets,and its structural identification and preliminary biological activity were carried out.METHODS:Unknown impurity in sirolimus tablets was isolated by silica gel column chromatography,and then purified by preparativeliquid chromatography technique.The structure was characterized by UV,IR,MS and NMR.Antifugi activity was tested by doubling dilution and antitumor activity was detected by sulforhodamine B assay.RESULTS:The purity of the unknown impurity of sirolimus tablets was 96.8%.It was identified as secorapamycin.CONCLUSION:Secorapamycin is the main impurity in the processing of sirolimus tablets,and its biological activity is lower than that of sirolimus.
作者
陈有钟
陈夏琴
陈晓明
刘颖
应加银
李夸良
黄捷
杨国新
Chen You-zhong;Chen Xia-qin;Chen Xiao-ming;Liu ying;Ying Jia-yin;LiKua-liang;Huang Jie;Yang Guo-xin(Fujian Institute of Microbiology,Fuzhou,Fujian 350007,China)
出处
《福建分析测试》
CAS
2024年第1期5-10,14,共7页
Fujian Analysis & Testing
基金
公益类科研院所专项项目(编号:2020R10050013)。
关键词
西罗莫司片
断雷帕霉素
分离纯化
结构表征
Sirolimus tablets
Secorapamycin
Separation and purification
Structural characterization
