摘要
药物中金属的残留危害着人类的身体健康,因此对药物中的残留金属含量进行检测已成为一项重要的检测项目。基于《中华人民共和国药典》(2015年版)方法,测定蒙脱石散中的5种金属元素(As、Cd、Cu、Pb和Mg),优化了微波消解仪和四极杆电感耦合等离子体质谱仪的工作参数。通过优化测定方法,检出限为As 0.05μg/L、Cd 0.1μg/L、Cu和Pb 1μg/L、Mg 100μg/L;方法定量限为As 0.02μg/g、Cd 0.03μg/g、Cu和Pb 0.33μg/g、Mg 33.33μg/g;重复性和稳定性的RSD均小于5%;加标回收率为As和Cd 70%~125%、Cu 75%~120%、Mg 92%~105%、Pb 80%~115%。对国内外8个批次不同品牌的蒙脱石散进行方法验证,评估结果表明,方法操作简单,结果准确可靠,适用于蒙脱石散样品中As、Cd、Cu、Pb和Mg的测定,可为蒙脱石散的质量评价和服用安全性提供理论依据和技术支持。
Metal residues in drugs are harmful to human health,so it has become an important test item to detect the metal residues in drugs.Base on Pharmacopoeia of the People’s Republic of China(2015),a method was established for the analysis of five metal elements(As,Cd,Cu,Pb,Mg)in montmorillonite powder,and the optimal working parameters of inductively coupled plasma mass spectrometry(ICP-MS)with microwave digestion were optimized in this paper.The instrumental parameters and microwave digestion conditions were optimized.Through the optimize,the limit of detection(LOD)was as As 0.05μg/L,Cd 0.1μg/L,Cu&Pb 1μg/L,Mg 100μg/L,respectively.The limit of quantity(LOQ)was as As 0.02μg/g,Cd 0.03μg/g,Cu&Pb 0.33μg/g,Mg 33.33μg/g,respectively;the repeatability and stability RSD of this method were not more than 5.0%(n=6).The recovery rate were between 70%—125%for As and Cd,75%—120%for Cu,80%—115%for Pb,92%—105%for Mg.The method was validated by eight batch different brands of montmorillonite powder from home and abroad,all the assessment results show that this method has the advantages of rapidness,simplicity,high sensitivity,good stability and accuracy.It can be applicable for the determination of As,Cd,Cu,Pb and Mg of montmorillonite powder samples.This method can provide theoretical basis and technical support for quality and security evaluation of montmorillonite powder.
作者
王红
杨浩
贾贵敏
王风贺
WANG Hong;YANG Hao;JIA Guimin;WANG Fenghe(School of Environment,Nanjing Normal University,Nanjing,Jiangsu 210023,China;School of Geography Science,Nanjing Normal University,Nanjing,Jiangsu 210023,China;Qixia Hospital of Nanjing,Nanjing,Jiangsu 210046,China)
出处
《中国无机分析化学》
CAS
2020年第6期8-13,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家自然科学基金资助项目(41673108)。
关键词
微波消解
ICP-MS
蒙脱石散
金属
检测
microwave digestion
inductively coupled plasma mass spectrometry
Montmorillonite powder
metals elements
detection
