LC-MS法分析头孢硫脒中的主要杂质

Identification of the main impurities of cefathiamidine by LC-MS

目的对国内四家头孢硫脒制剂产品进行检测,确证超过报告限度(>0.05%)杂质的结构。方法采用HPLC法、LC-MS法及NMR法对头孢硫脒进行了强制降解杂质研究、长期留样杂质研究、杂质谱研究。结果存在四个超过报告限度的杂质,降解杂质为去乙酰头孢硫脒和头孢硫脒内酯,其他杂质为7-溴乙酰胺头孢烷酸(7-BCA)、头孢硫脒Δ2异构体。结论为头孢硫脒的质量控制和稳定性研究提供了重要依据。

Objective To identify the structure of impurities beyond the reports limits（ 〉 0. 05%） ,cefathiamidine products of our company and three domestic companies were detected. Methods The forced degradation experiments, long term retention samples and spectroscopy for impurities in cefathiamidine were respectively investigated by HPLC, LC - MS and NMR. Results Four impurities were detected exceeding the report limits,in which deacetylation of cefathiamidine and cefathiamidine lactone were degradation products and the other two were 7 - bromoacetamide cephalosporanic acid （ 7 - BCA ） and △2 isomer of cefathiamidine. Conclusion The results were useful to quality control and stability studies for cefathiamidine.