克林霉素磷酸酯注射液中10种元素杂质测定方法的建立  

A method for the determination of 10 kinds of elemental impurities in clindamycin phosphate injection

作　　者：蒋大圆 Jiang Dayuan(Pharmacy faculty,Anhui Medical College,Hefei,Anhui,230601,China)

机构地区：[1]安徽省医学高等专科学校药学院,安徽合肥230601

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)。

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.

关 键 词：克林霉素磷酸酯注射液 元素杂质 电感耦合等离子体质谱 方法学验证 

分 类 号：R917[医药卫生—药物分析学]