ICP-MS法测定注射用奈达铂及其原辅料中23种元素杂质的含量  

Determination of 23 elemental impurities in nedaplatinfor injection,nedaplatin and excipients by ICP-MS

作　　者：黄晓春 侯金凤 刘琦 刘照振 刘海涛 车宝泉 HUANG Xiaochun;HOU Jinfeng;LIU Qi;LIU Zhaozhen;LIU Haitao;CHE Baoquan(Beijing Institute for Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China)

机构地区：[1]北京市药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中国药品标准》2024年第6期584-589,共6页Drug Standards of China

摘　　要：目的:建立电感耦合等离子体质谱(ICP-MS)法测定注射用奈达铂中砷(As)、镉(Cd)、汞(Hg)、铅(Pb)、银(Ag)、铬(Cr)、铜(Cu)等23种元素杂质含量。方法:样品直接溶解进样,采用ICP-MS技术,建立上述23种元素杂质的含量测定方法,并进行相关方法学验证。结果:上述23种元素杂质的响应值与质量浓度均呈良好的线性关系(r≥0.99)、重复性试验的RSD小于9%(n=6)、回收率在94%~116%(n=9)之间,均满足方法学验证的要求。国内4家企业的注射用奈达铂制剂及其原辅料共16批样品中的23种元素杂质含量均低于ICH Q3D限度的30%。结论:建立的ICP-MS方法操作简便,专属性强、灵敏精密准确;可为铂类抗肿瘤药物的原辅料和制剂中23种元素杂质检测和控制提供参考。Objective:To establish an ICP-MS method for the determination of 23 potential risk elemental impurities including As,Cd,Hg,Pb,Co,Ni,V,Ag,Au,Ir,Os,Pd,Rh,Ru,Se,Tl,Ba,Cr,Cu,Li,Mo,Sb,Sn in nedaplatin for injection,nedaplatin and excipients.Methods:Inductively coupled plasma mass spectrometry(ICP-MS)was used to establish a method for the contents of 23 elemental imputities in nedaplatin for injection,nedaplatin and excipients,and relevant methodological validation were carried out.The samples were pretreated by directly dissolution.Results:The method simultaneously determined 23 elemental impurities.The response values of the 23 elemental impurities showed a good linear relationship with their mass concentrations(r≥0.99).The relative standard deviations(RSDs)of the repeatability tests were less than 9%(n=6),and the average recovery rates ranged from 94%to 116%(n=9),which all met the requirements of methodological validation.The contents of 23 elemental impurities in total 16 batches from 4 manufacturers of nedaplatin for injection were all below 30%of the limits specified by ICH Q3D.Conclusion:The established ICP-MS method is simple,sensitive,accurate,and has good specificity and repeatability.It can be used as a quality control detection method for 23 elemental impurities in the platinum based anti-tumor drug substances and products.

关 键 词：元素杂质 注射用奈达铂 ICP-MS 法 风险评估 

分 类 号：R921.2[医药卫生—药学]