摘要
目的:建立ICP-MS法检测葡甲胺原料中10种元素杂质的方法。方法:以密闭高压微波消解法处理样品,采用ICP-MS法测定1类元素杂质砷(As)、镉(Cd)、汞(Hg)、铅(Pb)、2A类元素杂质钴(Co)、镍(Ni)、钒(V)、3类元素杂质锂(Li)、锑(Sb)、铜(Cu)的含量,并以全定量方式定量。结果:各元素杂质线性相关系数r均大于0.997;加样回收率在93.6%~116.8%,回收率RSD均低于7.4%;精密度RSD均低于5.4%;11批样品中镍元素含量低于ICH Q3D(R2)元素指导原则中2A类元素杂质的口服用每日允许暴露量(PDE),但高于注射用PDE;其余9种元素杂质含量均低于该指导原则中1类、2A、3类元素杂质的口服及注射用PDE。结论:该方法灵敏度高,精密度良好,能够准确地测定葡甲胺中1类、2A、3类元素杂质的含量;9批葡甲胺存在镍元素残留较高的风险。
Objective:To establish an ICP-MS method for the determination of 10 elemental impurities in meglumine(APIs).Methods:The samples were processed by closed high-pressure microwave digestion,and the contents of the Class 1 elemental impurities arsenic(As),cadmium(Cd),mercury(Hg)and lead(Pb),the Class 2A elemental impurities cobalt(Co),nickel(Ni)and vanadium(V),and the Class 3 elemental impurities lithium(Li),antimony(Sb)and copper(Cu)were detected by ICP-MS with total quantification.Results:The linear correlation coefficients(r)of each elemental impurity were greater than 0.997.The recoveries of the spiked samples ranged from 93.6%to 116.8%with RSD values of the recoveries lower than 7.4%.RSD values of the precision were lower than 5.4%.The content of nickel in 11 batches of the samples was lower than the permissible daily exposure(PDE)of the impurities of the elements of category 2A in the elemental guideline of ICH Q3D(R2)for oral use but higher than that of PDE of the impurities of category 2A for injection.Conclusion:The method is sensitive and precise enough to accurately determine the levels of Class 1,2A and 3 elemental impurities in meglumine.Nine batches of meglumine were found to have a high risk of nickel residue.
作者
赖俊敏
李志芳
曾敏珊
章娟
严小红
LAI Junmin;LI Zhifang;ZENG Minshan;ZHANG Juan;YAN Xiaohong(Guangzhou Institute for Drug Control,Guangzhou 510160,China)
出处
《中国药品标准》
CAS
2024年第5期452-457,共6页
Drug Standards of China
基金
国家药典委员会国家药品标准修订研究课题(2020Y009)。
