文献类型：期刊文献

中文题名：9-(E)-红霉素A肟杂质的分离与鉴定

英文题名：Separation and identifi cation of the inpurity of 9-(E)-oxime erythromycin A

作者：孟祥燕[1,2];李娜[1];彭凤[1];刘瑶[1];黄鑫[1];沈永淼[1]

机构：[1]绍兴文理学院化学化工学院;[2]浙江震元制药有限公司

年份：2016

卷号：41

期号：4

起止页码：280

中文期刊名：中国抗生素杂志

外文期刊名：Chinese Journal of Antibiotics

收录：CSTPCD、、北大核心2014、Scopus、北大核心、CSCD_E2015_2016、CSCD

基金：国家自然科学基金(No.NSFC 21202101)

语种：中文

中文关键词：红霉素A肟杂质;红霉素E肟;柱层析分离;结构鉴定;抗菌活性

外文关键词：Inpurity of oxime erythromycin A; Oxime erythromycin E; Column chromatography separation; Structure characterization; Antimicrobial activity

中文摘要：目的分离、纯化HPLC图谱中紧跟着9-(E)-红霉素A肟的一个未知的杂质,并鉴定它的化学结构。方法通过柱层析色谱法和重结晶法分离该杂质,然后通过1H-NMR、MS、X-射线单晶衍射确定了该杂质的结构。结果实验最终确定了该杂质最佳的分离条件:流动相为CHCl3:C2H5OH:NH4OH=10.0:1.2:0.1,重结晶的溶剂为氯仿和丙酮(V:V=7:3)。并用双倍稀释法对红霉素A肟和杂质红霉素E肟进行了抗菌活性研究。结论未知杂质为红霉素E的E式肟化产物,红霉素E肟的抗菌活性远低于红霉素A肟。

外文摘要：Objective To separate and purify an impurity which is followed by 9-（E）-oxime erythromycin A observed on HPLC analysis. Methods This impurity is separated by column chromatography and recrystallization method, and the structure of this unknown impurity is determined by 1H NMR, MS, X-ray crystallography. Results The optimal column chromatography separation conditions of this impurity is as follows： the volume ratio of chloroform, ethanol and ammonia water is 10.0：1.2：0.1, and the recrystallization solvent is chloroform and acetone（V： V=7：3）. The antibacterial activity of erythromycin A oxime and erythromycin E oxime were determined with double dilution method. Conclusion This unknown impurity is the oximation products of erythromycin E and the antibacterial activity of erythromycin E oxime is far lower than that of erythromycin A oxime.