超级微波消解-电感耦合等离子体质谱法-电子稀释EDR技术同时测定苍术中的常量和微量元素  

Simultaneous Determination of Macro and Trace Elements in Atractylodes by Super Microwave Digestion-ICP-MS-Electron Dilution-EDR Technology

作　　者：周文梅 杨颖 李亚维 卢洋 宫艳艳 周翔 ZHOU Wenmei;YANG Ying;LI Yawei;LU Yang;GONG Yanyan;ZHOU Xiang(Lianyungang Testing Center for Food and Drug Control,Lianyungang 222006,China)

机构地区：[1]连云港市食品药品检验检测中心,江苏连云港222006

出　　处：《品牌与标准化》2024年第6期1-6,共6页

基　　金：江苏省市场监督管理局重点科研项目(KJ2022046);江苏省市场监督管理局技术能力提升项目(NL2023047)。

摘　　要：目的:建立超级微波消解-电感耦合等离子体质谱法-电子稀释EDR技术,实现中药材苍术中的常量和微量元素含量的同时测定。方法:超级微波消解的高效消解效率结合HNO_(3)-H_(2)O_(2)-HF酸消解体系消解样品,利用电感耦合等离子体质谱法-电子稀释EDR技术进行常量和微量元素的同时检测。对所建立的方法进行测量范围、线性关系、检出限等方法学验证。结果:不同元素在质量浓度0~20.0μg·mL^(-1)范围内线性关系良好,相关系数为0.999412~0.999996,检出限均小于0.15 mg·kg^(-1),定量限均小于0.5 mg·kg^(-1),样品的精密度为0.56%~0.97%,重复性为0.85%~1.43%,回收率为89.25%~109.71%,均表明方法的准确度和正确度高,样品的稳定性测试表明样品在48 h内具有良好的稳定性。结论:本方法准确、简便、高效,适合批量植物根、茎、叶类样品,特别是中药材样品的元素含量测定,能够实现不同含量元素同时快速测定,为科学高效地评价中药材中常量、微量元素含量提供数据参考。Objective:To establish a super microwave digestion inductively coupled plasma mass spectrometry(ICP-MS)electron dilution EDR technique for simultaneous determination of constant and trace element contents in traditional Chinese medicine Atractylodes macrocephala.Methods:The high digestion efficiency of super microwave digestion was combined with the HNO_(3)-H_(2)O_(2)-HF acid digestion system to digest samples of Atractylodes,and ICP-MS-electron dilution-EDR technology was used to detect major and trace ements simultaneously.Conduct methodological verification on the measurement range,linear relationship,detection limit,etc.of the established method.Results:The different elements have a good linear relationship in the mass concentration 0~20.0μg·mL^(-1),the correlation coefficient is 0.999412~0.999996,the detection limits are less than 0.15 mg·kg^(-1),and the quantitation limits are less than 0.5 mg·kg^(-1),the precision of the samples are 0.56%~0.97%,the repeatability of the method are 0.85%~1.43%,and the recovery rate are 89.25%~109.71%,all indicating that the accuracy and correctness of this method are high.The stability test of the sample shows that the sample have good internal stability within 48 hours.Conclusion:This method is accurate,simple and efficient,and is suitable for the determination of element content in plant roots,stems and leaves,especially Chinese herbal medicine samples.It can achieve simultaneous and rapid determination of elements with different contents,and provide data reference for the scientific and efficient evaluation of the content of major and trace elements in Chinese herbal medicines.

关 键 词：超级微波 电感耦合等离子体质谱法 电子稀释EDR 元素 苍术 中药材 

分 类 号：O657.63[理学—分析化学] R284.1[理学—化学]