超级微波消解-电感耦合等离子体质谱法同时检测羟苯乙酯中9种元素杂质  

Simultaneous Detection of 9 Elemental Impurities in Ethylparaben by Ultra Microwave Digestion and Inductively Coupled Plasma Mass Spectrometry

作　　者：蔡立荣 周斌 梁晟 舒海平 谭跃 李昌亮 刘雁鸣 CAI Li-rong;ZHOU Bin;LIANG Shen;SHU Hai-ping;TAN Yue;LI Chang-liang;LIU Yan-ming(Hunan Institute for Drug Control,NMPA Key Laboratory for Pharmaceutical Excipients Engineering Technology Research,Hunan Changsha 410001;Hunan Warrant Pharmaceutical Co.,Ltd.,Hunan Changsha 410006,China)

机构地区：[1]湖南省药品检验检测研究院,国家药监局药用辅料工程技术研究重点实验室,湖南长沙410001 [2]湖南华纳大药厂股份有限公司,湖南长沙410006

出　　处：《广州化工》2024年第15期51-53,75,共4页GuangZhou Chemical Industry

基　　金：湖南省自然科学基金科药联合基金资助项目(2023JJ60105、2023JJ60106)。

摘　　要：建立超级微波消解和电感耦合等离子体质谱的方法并严格按照法规要求进行方法学验证。参考ICH Q3D要求采用所建方法对多个厂家的多批次羟苯乙酯中的1类、2A类以及其他元素Fe和Zn共9种元素进行检测,以控制阈值方法评估羟苯乙酯用于口服制剂时元素杂质的残留风险。结果所建立方法线性、检测限、定量限、准确度、精密度均符合法规要求,各元素定量限均小于控制阈值,实测数据显4个厂家14批样品中Cd、Hg、Zn的含量均低于定量限,Pb、As、Co、V、Ni、Fe 6种元素均高于定量限,但均未超过控制阈值,表明羟苯乙酯用于口服制剂中元素杂质残留风险较低。A method using ultra microwave digestion and ICP-MS was established and validatedstrictly in accordance with regulatory requirements.Following the principles of ICH Q3D guidelines,this method was applied to detect nine elements,including Class 1,Class 2A,as well as Fe and Zn,in multiple batches of ethylparaben from various manufacturers.The control threshold approach was used to evaluate the residual risk of elemental impurities in ethylparaben when used in oral formulations.The results demonstrated that the method's linearity,detection limit,quantification limit,accuracy and precision all met regulatory standards,with quantification limits for each element being below the control threshold.The measured data revealed that the contents of Cd,Hg and Zn in 14 batches from 4 manufacturers were all below the quantification limits,while Pb,As,Co,V,Ni,and Fe were above the quantification limits but did not exceed the control threshold.It was indicated that the risk of residual elemental impurities in ethylparaben used in oral formulations is relatively low.

关 键 词：药用辅料 羟苯乙酯 元素杂质 ICH Q3D 风险评估 

分 类 号：R917[医药卫生—药物分析学] R951[医药卫生—药学]