HPLC-ICP-MS法测定毛毛鱼中无机砷的不确定度评定

Evaluation of uncertainty in determination of inorganic arsenic in aquatic products of tassle filefish by high performance liquid chromatography-inductively coupled with plasma mass spectrometry

采用GB 5009.11-2014 《食品安全国家标准食品中总砷及无机砷的测定》中液相色谱-电感耦合等离子体质谱法测定毛毛鱼中的无机砷含量,参照CNAS-GL006《化学分析中不确定度的评估指南》和JJF1059.1-2012《测量不确定度的评定与表示》建立数学模型,对毛毛鱼中As(III)、As(V)的精密度、回收率进行验证,同时对试验过程中带来的不确定度分量进行了来源分析和评定。试验结果表明:当毛毛鱼中无机砷含量为0.096mg/kg时,无机砷i-As在95%的置信区间下扩展不确定度为0.007,测量过程中的不确定度最主要来源为校准曲线拟合和样品加标回收率。

The uncertainty evaluation in the determination of inorganic arsenic in tassle filefish by using High Performance Liquid Chromatography-Inductively Coupled with Plasma Mass Spectrometry was investigated,based on the GB 5009.11-2014"national food safety standards on the determination of total arsenic and inorganic arsenic in food".A mathematical model was established,referring to CNAS-GL006 Guidelines for"the Assessment of uncertainty in Chemical Analysis and JJF 1059.1-2012 Evaluation and Expression of Measurement Uncertainty".The precision and recovery of As(III)and As(V)in maomile fish were verified.Meanwhile,the sources of uncertainty measurement of the experiment were analyzed and evaluated.The results showed that the extended uncertainty of inorganic arsenic,i-As,was 0.007 with95%confidence interval,when the content of inorganic arsenic in tassle filefish was 0.096 mg/kg.The main factors influencing this determination uncertainty were found to be the calibration curve and recovery rate.