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Determination of sub-ng g~(-1) levels of total inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry after pre-concentration

机译:浓缩后氢化物发生原子吸收光谱法测定食品中总无机砷和硒的亚ng g〜(-1)

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摘要

A new and simple ultrasonic-assisted extraction (UAE) procedure was developed for the determination of inorganic arsenic and selenium in foods by hydride-generation atomic absorption spectrometry (HG-AAS). The various analytical variables affecting complex formation and extraction efficiency were investigated and optimised. The method is based on selective complex formation of As(lll) and Se(IV) in the presence of excess As(V) and Se(VI) with toluidine red in the presence of tartaric acid at pH 4.5, and then extraction of the resulting condensation products into the micellar phase of non-ionic surfactant, polyethylene glycol dodecyl ether, Brij 35. Under optimised conditions, good linear relationships were obtained in the ranges of 4-225 and 12-400 ng I~(-1) with limits of detection of 1.1 and 3.5 ng l~(-1) for As(lll) and Se(IV), respectively. The repeatability was better than 3.9% for both analytes (n = 10, 25 ng I~(-1)) while reproducibility ranged from 4.2% to 4.8%. The recoveries of As(lll) and Se(IV) spiked at 25-100 ng I~(-1) were in the range of 94.2-104.8%. After pre-concentration of a 5.0 ml sample, the sensitivity enhancement factors for As(lll) and Se(IV) were 185 and 140, respectively. Accuracy was assessed by analysis of two standard reference materials (SRMs) and spiked recovery experiments. The method was successfully applied to the accurate and reliable determination of total As and total Se by HG-AAS after pre-reduction with a mixture of L-cysteine and tartaric acid. Finally, the method was shown to be rapid and sensitive, with good results for extraction, pre-concentration and determination of total As and Se contents (as As(lll) and Se(IV)) from food samples.
机译:建立了一种新的简单的超声波辅助萃取(UAE)程序,用于氢化物发生原子吸收光谱法(HG-AAS)测定食品中的无机砷和硒。研究和优化了影响复合物形成和提取效率的各种分析变量。该方法是基于在过量的As(V)和Se(VI)存在下,甲苯胺红,在酒石酸的pH 4.5下选择性复合形成As(III)和Se(IV),然后萃取生成的缩合产物进入非离子表面活性剂的胶束相,聚乙二醇十二烷基醚,Brij35。在优化条件下,在4-225和12-400 ng I〜(-1)范围内获得了良好的线性关系As(III)和Se(IV)的检测分别为1.1和3.5 ng l〜(-1)。两种分析物(n = 10,25 ng I〜(-1))的重复性均优于3.9%,而重现性介于4.2%至4.8%之间。加标浓度为25-100 ng I〜(-1)的As(III)和Se(IV)的回收率在94.2-104.8%的范围内。预浓缩5.0 ml样品后,As(III)和Se(IV)的灵敏度增强因子分别为185和140。通过分析两种标准参考物质(SRM)和加标回收率实验来评估准确性。该方法成功地用于L-半胱氨酸和酒石酸的混合物预还原后,通过HG-AAS准确,可靠地测定总砷和总硒。最后,该方法显示了快速,灵敏的效果,在食品样品中总砷和硒含量(As(III)和Se(IV))的提取,预浓缩和测定方面均取得了良好的结果。

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