摘要
目的分离HPLC图谱中紧邻罗红霉素杂质G后洗脱的1个未知杂质(罗红霉素杂质G'),并对其化学结构进行鉴定。方法通过制备液相色谱分离该杂质,然后通过^(1)H-NMR、HRMS、^(13)C-NMR以及NMR二维相关谱等技术确定该杂质的结构。结果确定了该杂质的最佳色谱分离条件:流动相为CH_(2)Cl_(2):CH_(3)OH:NH_(4)OH(50:1:1)。结论未知杂质为红霉素E的衍生化产物,且具有和罗红霉素相当的抗菌活性。
Objective To separate an impurity which is followed by roxithromycin impurity G observed on HPLC analysis.Methods This impurity is separated by liquid chromatography method,and the structure is determined by ^(1)H NMR、HRMS、^(13)C NMR、2D NMR.Results The optimum liquid chromatography separation conditions of this impurity is as follows:The volume ratio of dichloromethane,methanol and ammonia water is 50:1:1.Conclusion This unknown impurity is a derivative product of erythromycin E and has the same antibacterial activity as roxithromycin.
作者
孟祥燕
冯传威
樊伟明
周炜祥
王建红
刘小睿
沈永淼
Meng Xiang-yan;Feng Chuan-wei;Fan Wei-ming;Zhou Wei-xiang;Wang Jian-hong;Liu Xiao-rui;Shen Yong-miao(Zhejiang Zhenyuan Pharmaceutical Co.,Ltd.,Shaoxing 312000;Department of Chemistry,School of Sciences,Zhejiang Sci-Tech University,Zhejiang Key Laboratory of Polymer Surface and Interface Science,Hangzhou 310018)
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2022年第4期361-365,共5页
Chinese Journal of Antibiotics
基金
国家自然科学基金(No.NSFC 21202101)
浙江理工大学科研启动基金(No.18062144-Y)。
关键词
罗红霉素杂质
红霉素E
结构鉴定
抗菌活性
Impurity of roxithromycin
Erythromycin E
Structure characterization
Antibacterial activity
