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Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

机译:酸浸萃取后电热原子吸收光谱法测定生物样品中的甲基汞

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摘要

An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 mu g g(-1) and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%.
机译:基于酸浸提取甲基汞到甲苯中,建立了一种高效,灵敏的测定生物样品中甲基汞的方法。通过电热原子吸收光谱法(ETAAS)测定有机相中的甲基汞。通过形成某些配合物和添加Pd-DDC改性剂,可以增强甲基汞信号,并提高可重复性。与双硫zone,半胱氨酸,1,10-菲咯啉和二乙基二硫代氨基甲酸酯的络合物相比,甲基汞与DDC的络合物在灵敏度和重现性方面产生了最佳的分析信号。通过修改参数,例如矿化温度,雾化温度和气体流速,可以优化方法性能。甲基汞测定的检出限为0.015μgg(-1),整个过程的相对标准偏差对于人牙齿样品(n = 5)为12%,对于头发样品(n = 5)为15.8%。使用NIES-13并用不同量的甲基汞加标样品来研究该方法的准确性。结果与标准值吻合良好,回收率为88-95%。

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