头孢克洛聚合物杂质的分析  

Analysis of polymer impurities of cefaclor

作　　者：张丹丹 赵浩然 刘文坤 李宁宁 常笑 陈德俊 Zhang Dandan;Zhao Haoran;Liu Wenkun;Li Ningning;Chang Xiao;Chen Dejun(Shandong Institute for Food and Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Public Service Platforms for Industrial Technology,Shandong Research Center of Engineering and Technology for Consistency Evaluation of Generic Drugs,Ji'nan 250101)

机构地区：[1]山东省食品药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,产业技术基础公共服务平台,山东省仿制药一致性评价工程技术研究中心,济南250101

出　　处：《中国抗生素杂志》2024年第3期333-340,共8页Chinese Journal of Antibiotics

摘　　要：目的对头孢克洛中聚合物杂质的结构进行初步鉴定,对其产生机理进行初步分析。方法以0.05 mol/L磷酸盐缓冲液(pH 8.0)为溶剂,室温放置4 d,制备头孢克洛强制聚合溶液;采用HPSEC法对强制聚合物溶液中各杂质进行分离,结合二维液相脱盐技术、柱切换-LC/MS^(n)技术,根据各杂质一级、二级精确质量信息及聚合机制,初步鉴定主峰前各杂质结构。结果对头孢克洛强制聚合溶液中的9个聚合物杂质结构进行初步解析,并初步分析其产生机理。结论强制聚合溶液可作为头孢克洛原料及制剂中聚合物杂质研究分析用系统适用性溶液。本研究中推测的聚合物杂质结构对头孢克洛原料及其制剂的杂质谱研究及质量控制有重要参考意义。Objective To identify the structures of polymer impurities in cefaclor raw materials.And the mechanisms of their production were analyzed.Methods The cefaclor forced-polymerization solution was prepared with 0.05 mol/L phosphate buffer(pH8.0)at room temperature for 4 days.The impurities in the forced-polymerization solution were separated by HPSEC method,and the structures of the impurities before the main peak were identified according to the primary and secondary precise mass information and the polymerization mechanism,combined with two-dimensional liquid desalination technology and column switching LC/MS~n technology.Results Preliminary elucidation was conducted on 9 polymer impurity structures present in the cefaclor forced-polymerization solution.Concurrently,an examination was conducted on their mechanisms of production.Conclusions The cefaclor forcedpolymerization solution can be used as suitable solution for the study and analysis of polymer impurities in cefaclor.The predicted polymer impurity structures in this study have important reference significance for the impurity profile study and quality control of cefaclor raw materials and their preparations.

关 键 词：头孢克洛 聚合物杂质 化学结构 柱切换-LC/MS^(n) 二维液相色谱 

分 类 号：R978.1[医药卫生—药品] R917[医药卫生—药学]