超声提取-电感耦合等离子发射光谱法测定中药材中12种主次量元素  

Determination of 12 major and minor elements in traditional chinese medicine by ultrasonic extraction inductively coupled plasma emission spectroscopy

作　　者：刘璐 张宁 金倩 孙凯茜 刘爱琴 康志娟 杨灵芝 宋娟娟 LIU Lu;ZHANG Ning;JIN Qian;SUN Kaiqian;LIU Aiqin;KANG Zhijuan;YANG Lingzhi;SONG Juanjuan(Hebei Provincial Geological Experimental Testing Center,Hebei Provincial Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071052)

机构地区：[1]河北省地质实验测试中心,河北省矿产资源与生态环境监测重点实验室,河北保定071052

出　　处：《化学分析计量》2025年第2期60-65,共6页Chemical Analysis And Meterage

基　　金：保定市科技计划项目(2341ZF166)。

摘　　要：建立超声提取-电感耦合等离子发射光谱法测定中药材中12种主次量元素。为解决中药材微波消解酸溶硅、铝、钛偏低且溶液中存在SiO_(2)沉淀问题,采用140~600℃逐步升温的灰化方法,LiBO_(2)碱熔融处理,超声加热浸提,利用电感耦合等离子体发射光谱法进行测定。LiBO_(2)与灰分质量比为4∶1,熔样温度为950℃,溶解时间为15min。针对引入的盐分,通过加大稀释倍数和基体匹配的方法抑制基体效应。钙、硅、磷、铝、硫、锰、钠、钛、锌、镁、钾、铁12种元素在各自质量浓度范围内与对应的光谱强度线性关系良好,相关系数均大于0.999,检出限为1.5~50μg/g。中药材标准物质中各元素测定结果的相对标准偏差均小于7.8%(n=12)。实际样品测定结果表明,该方法具有难熔元素多元素同时分析、准确度和精密度高的特点。A method for the determination of 12 major and minor elements in Chinese medicinal materials by ultrasonic extraction-inductively coupled plasma emission spectrometry was established.In order to solve the problem of low acid soluble Si,Al,Ti and SiO_(2) precipitation in the solution of microwave digestion of Chinese medicinal materials,the ashing method of gradual heating at 140-600℃,LiBO_(2) alkali fusion treatment,ultrasonic heating extraction,and determination by inductively coupled plasma emission spectrometry(ICP-OES)were used.The mass ratio of LiBO_(2) to ash was 4:1,the melting temperature was 950℃,and the melting time was 15 min.For the introduced salt,the matrix effect was suppressed by increasing the dilution ratio and matrix matching.The 12 elements of Ca,Si,P,Al,S,Mn,Na,Ti,Zn,Mg,K and Fe had a good linear relationship with the corresponding spectral intensity in their respective mass concentration ranges.The correlation coefficients of the standard curves were all greater than 0.999.The detection limits of each element were 1.5-50μg/g.The relative standard deviations of the determination results of each element in ginseng and astragalus standard materials were less than 7.8%(n=12).The actual sample determination results show that the method has the characteristics of simultaneous analysis of refractory elements,high accuracy and precision.

关 键 词：中药材 偏硼酸锂 碱熔 电感耦合等离子体发射光谱法 

分 类 号：O657.3[理学—分析化学]