International Atomic Energy Agency, Department of Nuclear Sciences and Applications, Environment Laboratories, 4 Quai Antoine 1er, MC 98000, Monaco.
International Atomic Energy Agency, Department of Nuclear Sciences and Applications, Environment Laboratories, 4 Quai Antoine 1er, MC 98000, Monaco.
Food Chem. 2015 Jun 1;176:367-75. doi: 10.1016/j.foodchem.2014.12.085. Epub 2014 Dec 29.
In this paper, we present a simple, fast and cost-effective method for determination of methyl mercury (MeHg) in marine samples. All important parameters influencing the sample preparation process were investigated and optimized. Full validation of the method was performed in accordance to the ISO-17025 (ISO/IEC, 2005) and Eurachem guidelines. Blanks, selectivity, working range (0.09-3.0ng), recovery (92-108%), intermediate precision (1.7-4.5%), traceability, limit of detection (0.009ng), limit of quantification (0.045ng) and expanded uncertainty (15%, k=2) were assessed. Estimation of the uncertainty contribution of each parameter and the demonstration of traceability of measurement results was provided as well. Furthermore, the selectivity of the method was studied by analyzing the same sample extracts by advanced mercury analyzer (AMA) and gas chromatography-atomic fluorescence spectrometry (GC-AFS). Additional validation of the proposed procedure was effectuated by participation in the IAEA-461 worldwide inter-laboratory comparison exercises.
本研究提出了一种简单、快速且经济高效的方法,用于测定海洋样品中的甲基汞(MeHg)。本文对影响样品制备过程的所有重要参数进行了考察和优化。方法的全面验证符合 ISO-17025(ISO/IEC,2005)和 Eurachem 指南的要求。对空白、选择性、工作范围(0.09-3.0ng)、回收率(92-108%)、中间精密度(1.7-4.5%)、溯源性、检出限(0.009ng)、定量限(0.045ng)和扩展不确定度(15%,k=2)进行了评估。本文还提供了对每个参数的不确定度贡献的估计以及测量结果可溯源性的证明。此外,通过使用高级汞分析仪(AMA)和气相色谱-原子荧光光谱法(GC-AFS)对相同的样品提取物进行分析,研究了该方法的选择性。通过参与国际原子能机构的 461 项全球实验室间比较研究活动,对所提出的方法进行了额外的验证。