注射用头孢美唑钠中10种ICH控制元素测定方法的建立  

A method for the determination of 10 elemental impurities in cefmetazole sodium for injection according to ICH requirement

作　　者：张凤妹 陈丹丹 顾霄 徐兵勇 王建 ZHANG Feng-mei;CHEN Dan-dan;GU Xiao;XU Bing-yong;WANG Jian(Zhejiang Institute for Food and Drug Control,Key Laboratory for Core Technology of Generic Drug Evaluation National Medical Product Administration,Hangzhou 310052,China;Zhejiang Heze Pharmaceutical Technology Co.,Ltd.,Hangzhou 310018,China)

机构地区：[1]浙江省食品药品检验研究院,国家药品监督管理局仿制药评价关键技术重点实验室,杭州310052 [2]浙江和泽医药科技股份有限公司,杭州310018

出　　处：《药物分析杂志》2023年第8期1446-1450,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：2022年度浙江省药监局科技计划项目(项目编号2022019和2021007)。

摘　　要：目的:根据ICH Q3D最新要求,建立同时测定注射用头孢美唑钠中10种元素杂质的方法。方法:样品经直接溶解并稀释后采用电感耦合等离子质谱分析,以硒(Se)、锗(Ge)、碲(Te)、镥(Lu)为内标,等离子功率1550 W,载气流量1.09 L·min^(-1)。结果:10种元素线性均良好(r均>0.999),检测限为0.0002~0.059 ng·mL^(-1),各浓度点平均回收率为90%~110%(n=3),重复性RSD为4%~10%(n=6)。5家企业12批样品中有3批测得镍(Ni)(0.1μg·mL^(-1)),其中1批测得锂(Li)(0.1μg·mL^(-1)),不同厂家的注射用头孢美唑钠中10种元素杂质含量均符合ICH规定。结论:本文应用的方法简单快速,灵敏度高,准确性好,可用于注射用头孢美唑钠中元素杂质的质量控制。Objective:To develop a method for simultaneous determination of 10 elemental impurities in cefmetazole sodium for injection according to the latest requirement of ICH Q3D.Methods:Samples were analyzed after direct dissolved and dilution by inductively coupled plasma mass spectroscopy(ICP-MS),with selenium(Se),germanium(Ge),tellurium(Te),and lutetium(Lu)as internal standards.RF power was set at 1550 W and carrier gas was set at 1.09 L·min^(-1).Results:The linear relationship for all elemental impurities were good(r>0.999),with a detection limit of 0.0002-0.059 ng·mL^(-1).The average recovery rate at each concentration point was 90%~110%(n=3),and the RSD were 4%-10%(n=6).Nickel(Ni)were detected at 0.1μg·mL^(-1)in 3 out of 12 batches of samples from five companies,and lithium(Li)was detected at 0.1μg·mL^(-1)in 1 batche.The contents of 10 elemental impurities in cefmetazole sodium for injection from different manufacturers comply with ICH requirement.Conclusions:The established method was simple,rapid,sensitive,accurate and can be used for the quality control of elemental impurities in cefmetazole sodium for injection.

关 键 词：注射用头孢美唑钠 电感耦合等离子质谱 ICH Q3D 元素杂质 定量分析 

分 类 号：R917[医药卫生—药物分析学]