ICP-MS测定氟比洛芬酯注射液中多种无机元素杂质含量  

Determination of Multiple Inorganic Elements in Flurbiprofen Axetil Injection by Inductively Coupled Plasma-mass Spectrometry

作　　者：张连义 郭常川 陈真 李文馨 杨书娟 窦艳丽 王雪 李琳 徐玉文 ZHANG Lian-yi;GUO Chang-chuan;CHEN Zhen;LI Wen-xin;YANG Shu-juan;DOU Yan-li;WANG Xue;LI Lin;XU Yu-wen(Shandong Institute for Food and Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Shandong Research Center of Engineering and Technology for Consistency Evaluation of Generic Drugs,Jinan 250101,China)

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山东省仿制药一致性评价工程技术研究中心,山东济南250101

出　　处：《食品与药品》2023年第5期420-425,共6页Food and Drug

基　　金：2022年国家药品抽检项目(编号:84)。

摘　　要：目的建立电感耦合等离子体质谱法(ICP-MS)测定氟比洛芬酯注射液中无机元素杂质的方法,并对抽检样品进行评价。方法根据ICH指导原则Q3D(R2)元素杂质指导原则,确定需要控制的元素种类,包括10种元素:Cd、Pb、As、Hg、Co、V、Ni、Li、Sb和Cu。建立ICP-MS内标校正的标准曲线法,并进行检出限、定量限、精密度、重复性、准确度方法验证。结果建立的内标校正的曲线法能够准确测定线性范围内的各元素杂质含量,线性相关系数r>0.999,精密度RSD≤4.2%,重复性RSD≤5.5%,各元素平均回收率94.39%~107.82%,定量限、检测限经验证结果良好。在73批样品中,部分样品检出Pb、As、Co、V和Ni元素,均未检出Cd、Hg、Li、Sb和Cu元素。结论该方法灵敏、准确、简便,样品预处理简单,可有效测定氟比洛芬酯注射液中的无机元素杂质含量。Objective To establish a method for the determination of inorganic element impurities in Flurbiprofen Axetil Injection by inductively coupled plasma-mass spectrometry(ICP-MS),and evaluate the samples.Methods According to the ICH guiding principle Q3D(R2)Guidelines for Elemental Impurities,the types of elements that needed to be controlled were determined,which included:Cd,Pb,As,Hg,Co,V,Ni,Li,Sb,Cu.A standard curve method of ICP-MS internal standard calibration was established and the detection limit,quantification limit,precision,repeatability,and accuracy were verified.Results The internal standard calibration curve method established could accurately determine the contents of element impurities within the linear range of each impurity.The linear correlation coefficient(r)was greater than 0.999,the RSD of precision was≤4.2%,the RSD of repeatability was≤5.5%,and the average recoveries of each element were 94.39%-107.82%.The quantitative limit and detection limit had been verified to be good.Among the 73 batches of samples,the five elements of Pb,As,Co,V,and Ni were detected in some samples,while Cd,Hg,Li,Sb,and Cu were not detected in all samples.Conclusion This method is sensitive,accurate and simple,with simple sample pretreatment.It can effectively determine the contents of inorganic element impurities in Flurbiprofen Axetil Injection.

关 键 词：氟比洛芬酯注射液 电感耦合等离子体质谱法 包材相容性 元素迁移 无机元素杂质 

分 类 号：R927[医药卫生—药学]