微波消解MPT-AES法测定玛卡中的微量金属元素  

Determination of trace metal elements in Marka by microwave digestion/MPT-AES method

作　　者：关皓天 吴限[1] 张金生[1] 宫晓杰[1] 李丽华[1] GUAN Hao-tian;WU Xian;ZHANG Jin-sheng;GONG Xiao-jie;LI Li-hua(College of Chemistry,Chemical Engineering and Environmental Engineering,Liaoning Shihua University,Fushun 113006,China)

机构地区：[1]辽宁石油化工大学化学化工与环境学部,辽宁抚顺113006

出　　处：《现代化工》2020年第11期234-237,共4页Modern Chemical Industry

基　　金：辽宁省科技厅大型仪器设备共享服务平台能力建设基金项目(20170006)。

摘　　要：建立了微波消解结合MPT-AES法测定中药玛卡中Ca、Fe、Zn、Cu、Cd、Pb的方法,样品经微波消解后,利用微波电感耦合等离子体炬发射光谱(MPT-AES)进行了测定,并对影响微波消解的因素和条件进行了考察,对MPT光谱仪的载气流量、工作气流量等仪器参数进行了优化选择,并且对酸效应和共存元素的影响也进行了实验,在最佳实验条件下得到Ca、Fe、Zn、Cu、Cd、Pb检出限依次为5.61、12.4、7.8、3.7、3.4、6.1 ng/m L,RSD(精密度)在0.3%~1.5%,加标回收方法检测出Ca的回收率区间为99%~101.5%,Fe的回收率在102%~104%,Zn的回收率区间在95.5%~97%,Cu、Cd、Pb的回收率分别在96.5%~98.5%、98%~104%、94%~96%。Microwave digestion combined with microwave inductively coupled plasma torch of emission spectrum( MPT-AES) method is established for determination of Ca,Fe,Zn,Cu,Cd and Pb in Marka,a traditional Chinese medicine. After the sample is digested by microwave,it is determined by MPT-AES,and the influence factors and conditions of microwave digestion are investigated. The parameters of MPT spectrometer,such as carrier gas flow and work gas flow are optimized,and the acid effect and the influence of coexisting elements are also investigated. Under the optimum experiment conditions,the detection limits for Ca,Fe,Zn,Cu,Cd,and Pb are 5. 61,12. 4,7. 8,3. 7,3. 4,and6. 1 ng·mL^-1,respectively,RSD( precision) is between 0. 3%-1. 5%,the recovery of Ca is in the range of 99%-101. 5%,that of Fe in the range of 102%-104%,that of Zn in the range of 95. 5%-97%,the recoveries of Cu,Cd,Pb in 96. 5%-98. 5%,98%-104% and 94%-96%,respectively.

关 键 词：微波消解 微波等离子体炬原子发射光谱法 精密度 加标回收率 

分 类 号：O657.31[理学—分析化学]