微波消解-电感耦合等离子体质谱法测定林蛙油中19种元素含量

Determination of 19 kinds of elements content in Oviductus ranae by microwave digestion-inductively coupled plasma mass spectrometry

中文关键词:  电感耦合等离子体质谱法  八级杆碰撞/反应池系统  林蛙油  微量元素

英文关键词:inductively coupled plasma mass spectrometry  eight-stage rod collision/reaction cell system  Oviductus ranae  trace elements

中文摘要:

      目的 建立了一种电感耦合等离子体质谱法(inductively coupled plasma mass spectrometry, ICP-MS)同步测定林蛙油中19种金属元素的分析方法。方法 采用HNO3-H2O2 (5:2, V:V)混合体系微波消解样品, 结合八极杆碰撞/反应池系统消除质谱干扰, 优化仪器参数以提高灵敏度和准确性, 内标法定量。结果 通过标准物质(GSB-28)验证及加标回收实验, 结果显示19种元素(钒、铬、锰、铁、钴、镍、铜、锌、镓、砷、硒、锶、银、镉、铯、钡、铊、铅、铀)的回收率为87.8%~108.6%, 相对标准偏差小于10%, 检出限为0.1~48.3 μg/kg。实际样品检测表明, 林蛙油中铁、锰、铜、锌、锶等元素含量较高, 而铬、砷、镉等元素含量较低。结论 该方法具有前处理简便、灵敏度高、稳定性好等优点, 适用于林蛙油中多种微量元素的快速同步检测, 为相关质量控制和标准制定提供技术支持。

英文摘要:

      Objective To establish an analytical method for the simultaneous determination of 19 kinds of metal elements in Oviductus ranae by inductively coupled plasma mass spectrometry (ICP-MS). Methods Samples were digested using a microwave-assisted digestion system with a HNO3-H2O2 (5:2, V:V) mixed acid system. Spectral interferences were eliminated using an eight-stage rod collision/reaction cell system, and instrument parameters were optimized to improve sensitivity and accuracy. Quantification was performed using the internal standard method. Results Method validation using certified reference material (GSB-28) and spiked recovery tests showed that the recoveries for the 19 kinds of elements (V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sr, Ag, Cd, Cs, Ba, Tl, Pb, U) ranged from 87.8% to 108.6%, with relative standard deviations less than 10%. The limits of detection ranged from 0.1 to 48.3 μg/kg. Analysis of actual samples indicated higher content of elements such as Fe, Mn, Cu, Zn and Sr, while levels of Cr, As and Cd were relatively low. Conclusion The established method is simple in sample preparation, highly sensitive and exhibits good stability. It is suitable for the rapid and simultaneous detection of multiple trace elements in Oviductus ranae, providing technical support for quality control and standard formulation.