MEKC和HPLC检测头孢噻吩钠的杂质谱  

Impurity profi ling of cefalotin sodium by MEKC and HPLC

作　　者：刘浩[1] 贾志强 

机构地区：[1]上海市食品药品检验所,上海201203 [2]苏州中联化学制药有限公司,苏州215212

出　　处：《中国抗生素杂志》2013年第12期921-927,共7页Chinese Journal of Antibiotics

基　　金：重大新药创制专项化学新药质量标准研究与评价技术平台(2011ZX09303-001)

摘　　要：目的针对现行药典HPLC系统的不足之处,分别采用优化后的反相HPLC系统和新建立的MEKC系统检测头孢噻吩钠的杂质谱。方法合成杂质A并采用ESI-MS、IR、1H-NMR和13C-NMR等对其进行结构确认;通过优化反相HPLC系统流动相的pH值和缓冲液浓度改善分离;建立MEKC系统和正相HPLC系统检测头孢噻吩钠的杂质谱。结果证实现行药典方法存在对头孢噻吩钠杂质A的误认和有关物质之间分离较差等缺陷;采用新建立的MEKC系统,发现头孢噻吩钠的市售品和对照品中均存在一个反相HPLC系统难以分离且含量最高可达1.5%的未知杂质。结论新建立的MEKC系统可对头孢噻吩钠的杂质进行更为有效而全面的检测。Objective Considering the shortcoming of the HPLC method included in current pharmacopeia, an optimized RP-HPLC system and a novel MEKC system was established to profile the impurities in cefalotin sodium. Methods Impurity A was synthetized and its structure was confirmed by ESI-MS, IR, 1H-NMR and 13C-NMR. The separation in the RP-HPLC system was improved through optimizing the pH value and buffer concentration of mobile phase. The impurities in cefalotin sodium was profiled with the new established MEKC system and NP- HPLC system. Results It was confirmed that current pharmacopeia has mistaken impurities A of cefalotin sodium and the separation among the related substances was poor. Utilizing the new established MEKC system, an unknown impurity with its content of as high as 1.5% was found in commercial products and chemical reference substances. The unknown impurity could not be separated by current RP-HPLC system. Conclusion The novel MEKC system was more suitable for profiling of impurities in cefalotin sodium.

关 键 词：MEKC HPLC 杂质谱检测 头孢噻吩钠 

分 类 号：O657.7[理学—分析化学] R978.11[理学—化学]