ICP-MS法测定消渴清颗粒原料药材中15种重金属和有害元素及其不确定度评估

目的：建立电感耦合等离子体质谱法（ICP-MS法）测定消渴清颗粒的5种原料药材苍术、蒲黄、知母、黄连和地锦草中15种重金属及有害元素含量，并对测定结果进行不确定度评估。方法：采用ICP-MS（KED模式）联合微波消解法，分析测定流程，建立数学模型，根据JJF1059.1-2012《测量不确定度的评定与表示》对测量结果的各不确定度来源进行分析和评估，并计算合成不确定度。结果：实验建立的15种重金属及有害元素检测方法具有良好的线性关系，且重复性和精确度良好，线性系数均大于0.992，RSD低于5.0%，加样回收率在87%~115%之间。其不确定度主要来源于曲线拟合和微波消解过程。15种重金属及有害元素含量的合成不确定度分别为V 2.93%，Cr 4.43%，Ni 2.65%，Cu 5.70%，As 6.92%，Mo 2.02%，Ru 1.76%，Rh 2.07%，Pd 9.39%，Cd 2.75%，Os 4.72%，Ir 1.41%，Pt 7.31%，Hg 3.29%，Pb 4.28%。结论：ICP-MS法对消渴清颗粒原料药材中15种重金属及有害元素的测量中，可通过优化曲线拟合及微波消解过程从而减小不确定度的值。

Objective:To establish a determination method of fifteen kinds of heavy metals and harmful elements in five raw materials (Atractylodis Rhizoma, Typhae Pollen, Anemarrhenae Rhizoma, Coptidis Rhizoma and Euphorbiae Humifusae Herba) of Xiaokeqing granules by ICP-MS, and to analyze the uncertainty.Methods:The microwave digest technique combined with ICP-MS (KED mode) was used to determinate the 15 kinds of heavy metals and harmful elements.Through establishment of the mathematical model, the main sources of the uncertainty resulted from the determination process were calculated and discussed by the method recommended by JJF1059.1-2012 ‘Evaluation and expression of uncertainty in measurement’.Results:The detection methods of 15 heavy metals and harmful elements established in the experiment had good linear relationship, good repeatability and accuracy.The linear coefficients were greater than 0.992 with RSDs less than 5.0%, and the recovery rates were between 87% and 115%.The uncertainty sources were mainly from the curve fitting and microwave digestion process.The uncertainties of the measurement by ICP-MS were 2.93% for V, 4.43% for Cr, 2.65% for Ni, 5.70% for Cu, 6.92% for As, 2.02% for Mo, 1.76% for Ru, 2.07% for Rh, 9.39% for Pd, 2.75% for Cd, 4.72% for Os, 1.41% for Ir, 7.31% for Pt, 3.29% for Hg and 4.28% for Pb.Conclusion:The uncertainties of fifteen kinds of heavy metals and harmful elements in five raw materials of Xiaokeqing granules determined by ICP-MS can be reduced by optimization of the curve fitting and microwave digestion process.

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