头孢美唑钠原料及制剂的聚合物研究  

Research on Polymers in the Raw Materials and Preparations of Cefmezole Sodium

作　　者：张夏 刘慧 姚尚辰 李进 宁保明 胡昌勤 ZHANG Xia;LIU Hui;YAO Shangchen;LI Jin;NING Baoming;HU Changqin(National Institutes for Food and Drug Control,Institute for Chemical Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院化学药品检定所,北京102629

出　　处：《中国药物警戒》2024年第11期1264-1269,1283,共7页Chinese Journal of Pharmacovigilance

基　　金：国家自然科学基金资助项目(81903731)。

摘　　要：目的建立头孢美唑钠原料和制剂中聚合物的分析方法,为其生产质控和有效监管提供参考。方法采用含挥发性缓冲盐的色谱系统结合梯度洗脱对头孢美唑聚合物进行分离,与质谱联用对聚合物进行快速定位和鉴定,采用二维液相色谱法确定聚合物在《中华人民共和国药典》有关物质方法中的位置,并考察高效凝胶色谱法和反相高效液相色谱法对头孢美唑聚合物分离的专属性。结果头孢美唑原料和制剂中存在二聚体,参比制剂和高浓度降解样品中不含聚合物。《中华人民共和国药典》方法能够同时对有关物质和二聚体进行控制。反相高效液相色谱法分离聚合物的专属性优于高效凝胶色谱法。结论采用的技术路径可为其他聚合物含量较低、定位较困难的头孢菌素类抗生素的聚合物研究提供参考。Objective To establish an analytical method for polymers in cefmetazole sodium raw materials and preparations,which can provide guidance for production quality control and effective supervision.Methods The reversed phase liquid chromatography system containing volatile buffer salt was used to separate the polymers in cefmetazole with gradient elution,and the polymers were quickly identified coupled with mass spectrometry.The location of the polymers under the chromatographic method of related substances in the Chinese Pharmacopoeia was obtained by two-dimensional liquid chromatography,and the specificity of the high performance gel chromatography and reverse-phase high performance liquid chromatography for the separation of polymers in cefmetazole was explored.Results There is one dimer present in the raw materials and preparations of cefmetazole,while the reference listed drugs and high concentration degradation samples do not contain polymers.The pharmacopoeial method can simultaneously control related substances and the polymer.Reversed-phase high performance liquid chromatography is superior to high performance gel chromatography in the specificity of separating polymers.Conclusion The adopted technical pathway can provide guidance for the research on polymers in other cephalosporin with low content and difficult identification.

关 键 词：头孢美唑钠 聚合物 高效凝胶色谱法 反相高效液相色谱法 二维液相色谱法 液质联用 

分 类 号：R917[医药卫生—药物分析学]