高效凝胶色谱联用质谱法快速鉴定盐酸头孢吡肟中的聚合物  

Rapid Identification of Polymers in Cefepime Hydrochloride by High Performance Gel Chromatography Coupled with Mass Spectrometry

作　　者：张夏[1] 刘颖[1] 李进[1] 宁保明[1] 胡昌勤[1] ZHANG Xia;LIU Ying;LI Jin;NING Bao-ming;HU Chang-qin(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《中国药物评价》2024年第5期352-357,共6页Chinese Journal of Drug Evaluation

摘　　要：目的:采用高效凝胶色谱法联用质谱法推断注射用盐酸头孢吡肟中聚合物的结构。方法:采用TSK gel G2000SWxl高效分子排阻色谱柱,以5 mM甲酸铵溶液-乙腈(95∶5)为流动相,流速为0.8 mL·min^(-1),检测波长为254 nm,柱温为25℃。在正离子模式下获取各聚合物杂质的质谱数据,结合头孢类抗生素聚合物的质谱裂解规律、降解反应原理,解析相关聚合物的结构。结果:推断出4种聚合物的化学结构,其中2个是头孢吡肟二聚体杂质,另外2个是三聚体杂质,其中三聚体杂质为首次报道。结论:采用高效凝胶色谱法联用质谱技术,可快速推断出注射用盐酸头孢吡肟中的聚合物的化学结构,可为其他头孢菌素聚合物的分离、鉴定及产品质量提高提供参考。Objective:To infer the structures of the polymers in cefepime hydrochloride for injection by high performance gel chromatography coupled with mass spectrometry.Methods:TSK gel G2000SWxl column was used,with 5 mM ammonium formate solution-acetonitrile(95∶5)as the mobile phase,flow rate of 0.8 mL·min^(-1),detection wavelength of 254 nm,and column temperature of 25℃.Mass spectrometry data of various polymers was obtained in positive ion mode,and the structures of polymers were analyzed based on the mass spectrometry fragmentation rules and degradation reaction rules of cephalosporin polymers.Results:The chemical structures of four polymers were inferred.Two of them were dimers,and other two were trimers,which were reported for the first time.Conclusion:The chemical structures of the polymers in cefepime hydrochloride for injection can be quickly inferred using high performance gel chromatography combined with mass spectrometry technology,which can provide guidance for the isolation and identification of polymers in other cephalosporins and their quality improvement.

关 键 词：注射用盐酸头孢吡肟 聚合物 高效凝胶色谱法 液质联用 头孢类抗生素 

分 类 号：R927.13[医药卫生—药学] R927.32