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Reference measurements of mercury species in seafood using isotope dilution inductively coupled plasma mass spectrometry

机译:使用同位素稀释电感耦合等离子体质谱法使用同位素稀释汞种类的参考测量

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Species-specific isotope dilution inductively coupled plasma mass spectrometry (SS ID ICP-MS) and high-performance liquid chromatography (HPLC) were used to obtain accurate and SI traceable results for methyl mercury in seafood samples such as clam, oyster and fish homogenate. The mass fractions of (62.3 +/- 2.3) mu g kg(-1), (5.44 +/- 0.36) mu g kg(-1) and (531 19) mu g kg(-1) were obtained for MeHg (as Hg) in IAEA-461, IAEA-470 and IAEA-476, respectively. Direct isotope dilution mass spectrometry was performed for total mercury content then the content of inorganic mercury in selected samples was obtained by calculation. It was found that the content of inorganic Hg in IAEA-461, IAEA-470, and IAEA-476 was as: 328 mu g kg(-1), 16 mu g kg(-1), and 62 mu g kg(-1), respectively. Mathematical modelling of analytical procedure and evaluation of all parameters influencing final results were adequate for validation of measurement procedure, establishing traceability and estimating expanded uncertainty. Developed procedures were successfully applied in the characterization process of fish homogenate candidate reference material and in the calculation of assigned values in the frame of IAEA-476 inter-laboratory comparison study. Compatibility between obtained results and those derived from the certification campaign, organized by International Atomic Energy Agency on the same sample matrix ( 2.6 % difference) further validated performed ID ICP-MS protocols.
机译:物种特异性同位素稀释电感耦合等离子体质谱(SS ID ICP-MS)和高性能液相色谱(HPLC)用于获得海鲜样品中甲基汞的精确且Si可追踪结果,例如蛤,牡蛎和鱼匀浆。 (62.3 +/- 2.3)mu g kg(-1),(5.44 +/- 0.36)mu g kg(-1)和(53119)mu g kg(-1)的质量级分,Mehg(在原子能机构-461,IAEA-470和IAEA-476中分别为HG)。直接同位素稀释质谱法进行总汞含量,然后通过计算获得所选样品中无机汞的含量。发现IAEA-461,IA-470和IAEA-476中无机Hg的含量为:328μgkg(-1),16μgkg(-1)和62μgkg( - 1)分别。影响最终结果的所有参数的分析程序和评估的数学建模是足以验证测量程序的验证,建立可追溯性和估算扩大不确定性。开发的程序在鱼均匀候选参考材料的表征过程中成功应用,并在实验室间比较研究框架中的指定值计算。获得的结果与源自认证活动的兼容性,由国际原子能机构上的相同样品矩阵(& 2.6%差异)进行了进一步验证的ICP-MS协议。

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