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微波消解-ICP-OES法检测湘产朱砂中重金属的含量
引用本文:蒋秋桃,;曾丽,;丁野,;马杰,;孙辉,;李洁,;李文莉.微波消解-ICP-OES法检测湘产朱砂中重金属的含量[J].中国药事,2014(11):1247-1251.
作者姓名:蒋秋桃  ;曾丽  ;丁野  ;马杰  ;孙辉  ;李洁  ;李文莉
作者单位:[1]中南大学化学化工学院,长沙410083; [2]中国农工民主党湖南省委员会;,长沙410083; [3]湖南省食品药品检验研究院,长沙410083;
基金项目:十二五“重大新药创制”科技重大专项课题(编号2014ZX09304-307-02)
摘    要:目的建立微波消解-电感耦合等离子体原子发射光谱法(ICP-OES)检测湘产朱砂中Cd、Cr、Cu、Pb的含量,为矿物药的重金属检测提供参考。方法通过对比湿法消解,优选出微波消解作为朱砂样品的前处理方法,结合电感耦合等离子体发射光谱法(ICP-OES)的分析手段,对湖南产的11批朱砂样品中重金属含量进行检测。结果方法的线性相关系数为0.999 8~1.000 0,检出限为0.18~5.54μg·L^-1,RSD为0.55%~3.20%,回收率为84.30%~108.36%,经方法学验证适合同时测定朱砂中Cd、Cr、Cu、Pb的含量。结论该方法简便、准确,可同时检测朱砂中重金属Cd、Cr、Cu、Pb的含量。

关 键 词:朱砂  硫化汞  微波消解  重金属  电感耦合等离子体原子发射光谱法(ICP-OES)

Rapid Determination of Contents of Heavy Metals in Cinnabar from Hunan by Microwave Digestion and ICP-OES
Institution:Jiang Qiutao,Zeng Li,Ding Ye,Ma Jie,Sun Hui,Li Jie,Li Wenli(1College of Chemistry and Chemical Engineering, Central South University, Changsha 410083; 2The Chinese Peasants' and Workers' Democratic Party Committee of Hunan Province; 3 Hunan Food and Drug Inspection Institute)
Abstract:Objective To determine the contents of heavy metals in cinnabar from Hunan province by means of microwave digestion and inductively coupled plasma optical emission spectrometer(ICP-OES),and provide references for determination of heavy metals in mineral drugs.Methods Microwave digestion was selected as the optimal pretreatment method for cinnabar samples by comparing with the wet digestion method and the contents of Cd,Cr,Cu and Pb were determined in 11 lots of cinnabar from Hunan province by ICP-OES.Results The linear correlation coefficient was 0.999 8-1.000 0.The value of detection limit(3σ)was 0.18-5.54μg·L^-1.The relative standard deviation in measurement was 0.55%-3.20%,and the rate of recovery of standard sample addition was 84.30%-108.36%.Method validation showed that this method was suitable for simultaneous determination of the contents of the above mentioned elements in cinnabar.Conclusion ICP-OES with microwave digestion is rapid,reliable and the method can be applied to determine heavy metals(Cd,Cr,Cu,Pb)in cinnabar.
Keywords:cinnabar  mercuric sulfide  microwave digestion  heavy metal  inductively coupled plasma optical emission spectrometer(ICP-OES)
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