Isolation and structure characterization of related impurities in etimicin sulfate by LC/ESI-MSn and NMR
Isolation and structure characterization of related impurities in etimicin sulfate by LC/ESI-MSn and NMR
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通过 LC/ESI-MSn 和 NMR 分离硫酸依替米星中的相关杂质并进行结构表征
DOI：
10.1016/j.jpba.2011.03.005
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发表时间：
2011-07-15
影响因子：
3.4
通讯作者：
Ye, Wencai
中科院分区：
文献类型：
--
作者：
Wang, Hao;Zhang, Zhijie;Ye, Wencai
硫酸依替米星是一种由庆大霉素Cla改造而成的半合成氨基糖苷类抗生素，对革兰氏阳性和革兰氏阴性细菌感染均有效。采用LC-ELSD和LC-ESI-MSN法对原料药中的10种杂质进行了检测。采用弱酸性阳离子交换树脂、CM-Sephadex和硅胶柱层析分离6种杂质。经LC/ES1-MSN和核磁共振分析鉴定为庆大霉素C1a(1)、1-N-乙基加拉胺(2)、2‘’-N-乙基庆大霉素C1a或6‘’-N-乙基庆大霉素C1a(3)、1-N-乙基-3‘-N-去甲基庆大霉素C2b(4)、3-N-乙基庆大霉素Cla(5)、6’-脱氨基-6‘-羟基庆大霉素(6)、1，3-N，N-二乙基庆大霉素(7)、1-N-乙基庆大霉素C2B(8)、2‘’或6‘’-N-乙基依替米星(9)，1，3-N，N-二乙基庆大霉素C1a(10)。10是一个新的氨基糖苷类化合物，本文首次报道了化合物5-7、10的H-1和C-13核磁共振数据。文中还讨论了杂质形成的可能机理。(C)2011年爱思唯尔。版权所有。
Etimicin sulfate is a semi-synthetic aminoglycoside which is modified from gentamicin Cl a, used as an antibiotic effective both to Gram-positive and Gram-negative bacteria infections. Ten impurities were detected in the bulk drug by LC-ELSD and LC-ESI-MSn. Weakly acidic cation exchange resin, CM-sephadex and silica gel column chromatography were used for the isolation of six impurities. Based on LC/ES1-MSn and NMR analysis, related impurities were characterized as gentamicin C1a (1), 1-N-ethyl garamine (2), 2 ''-N-ethyl gentamicin C1a, or 6 ''-N-ethyl gentamicin Cl a (3), 1-N-ethyl-3'-N-demethyl gentamicin C2b (4), 3-N-ethyl gentamicin Cl a (5), 6 ''-deamino-6 ''-hydroxyl etimicin (6), 1,3-N, N-diethyl garamine (7), 1-N-ethyl gentamicin C2b (8), 2 '' or 6 ''-N-ethyl etimicin (9), 1,3-N, N-diethyl gentamicin C1a (10). 10 is a new aminoglycoside, the H-1 and C-13 NMR data of compounds 5-7, 10 are first reported in the paper. The possible mechanism for the formation of impurities is also discussed. (C) 2011 Elsevier By. All rights reserved.