摘要
目的建立电感耦合等离子体质谱法(ICP-MS)同时测定克林霉素磷酸酯注射液中Cd、Pb、As、Hg、Co、V、Ni、Li、Sb和Cu 10种杂质元素。方法样品经稀释后,以Be、Sc、Ge、Rh、Bi为内标,采用ICP-MS分析,测量模式为碰撞池模式。对所建立的方法进行方法学验证。结果10种元素的标准曲线均大于0.999;各浓度点元素平均回收率在94%-107%范围内;检出限在0.0001-0.04 ng·ml^(-1)间;重复性(n=6)和中间精密度(n=12)的RSD均小于2.0%;均满足USP通则<233>和EP10.0<2.4.20>方法学验证的要求。样品检测的结果均远小于ICH Q3D元素杂质指南中各元素杂质的每日允许暴露量。结论本研究建立的ICP-MS方法简单快速,基质干扰小,灵敏度高,具有良好的准确度和精密度,适用于克林霉素磷酸酯注射液中10种元素杂质的质量控制。
Objective To develop a method for simultaneous determination of 10 elemental impurities(Cd,Pb,As,Hg,Co,V,Ni,Li,Sb and Cu)in clindamycin phosphate injection based on Inductively coupled Plasma Mass Spectrometry(ICP-MS).Methods Samples were analyzed after direct dilution by inductively coupled plasma mass spectroscopy(ICP-MS)with Be,Sc,Ge,Rh,and Bi as internal standard.The measurement mode was collision cell mode.The established method was validated.Results The linear relationship for all elemental impurities was good(r>0.999).The average recoveries were between 94%-107%(n=9).Detection limits were between 0.0001-0.04 ng mL^(-1).The RSD of repeatability(n=6)and intermediate precision(n=12)were less than 2.0%,respectively.The results meet the validation requirements of USP general chapter<233>and EP 10.0 methods of analysis<2.4.20>.The contents of 10 elemental impurities in clindamycin phosphate injection were much less than the permitted daily exposure(PDE)of elemental impurities in ICH Q3D Guideline.Conclusions The established ICP-MS method is simple,rapid,sensitive,has low matrix interference and good accuracy and precision.This method is applicable for the quality control of 10 elements in clindamycin phosphate injection.
作者
蒋大圆
Jiang Dayuan(Pharmacy faculty,Anhui Medical College,Hefei,Anhui,230601,China)
出处
《齐齐哈尔医学院学报》
2023年第10期962-966,共5页
Journal of Qiqihar Medical University
基金
安徽省医学高等专科学校科研项目(YZ2020HX004)。
