首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Feasibility study of ion-chromatography microwave assisted on-line species conversion hydride generation atomic absorption spectrometry for selenium speciation analysis of biological material
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Feasibility study of ion-chromatography microwave assisted on-line species conversion hydride generation atomic absorption spectrometry for selenium speciation analysis of biological material

机译:离子色谱微波辅助在线物种转化氢化物发生原子吸收光谱法对生物材料中硒形态分析的可行性研究

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摘要

A method for selenium speciation based on ion-chromatography (IC) microwave (MW) assisted on-line species conversion hydride generation (HG) atomic absorption spectrometry (AAS) is described. The conversion of selenium species into selenite was achieved by using hydrobromic acid and bromate. A potential interferent originating from the reagents was identified. Multivariate optimization of the IC-MW-HGAAS system was undertaken and the results show that the HBr/BrO_3- ration is a very important parameter, which should be carefully controlled both to obtain a high conversion efficiency and to diminish the interferent. The feasibility of the IC-MW-HGAAS system for real samples is demonstrated by the application of selenium speciation in extracts of the certified reference material CRM 402. The system is shown to be sensitive to interferences but the detection capability is good, relative detection limits being 1.0-1.6 ng g~(-1) (based on a 50 #mu#L injection volume) for the species investigated: selenomethionine, selenite, selenate and selenocystine. Selenate was quantified in the CRM 402 extract at a level of approx=1.5 #mu#g g~(-1) corresponding to approx=22% the total selenium content in the material. The method described is concluded to be operationally defined because of the extraction procedure used.
机译:描述了一种基于离子色谱法(IC)微波(MW)辅助在线物种转化氢化物发生(HG)原子吸收光谱法(AAS)的硒形态分析方法。通过使用氢溴酸和溴酸盐将硒物质转化为亚硒酸盐。确定了源自试剂的潜在干扰物。对IC-MW-HGAAS系统进行了多变量优化,结果表明HBr / BrO_3-比率是一个非常重要的参数,应仔细控制HBr / BrO_3-比率以获得高转换效率并减少干扰物。硒形态分析法在经认证的参考材料CRM 402的提取物中的应用证明了IC-MW-HGAAS系统用于实际样品的可行性。该系统显示出对干扰敏感,但检测能力良好,相对检测极限对于所研究的物种:硒蛋氨酸,亚硒酸盐,硒酸盐和硒代胱氨酸为1.0-1.6 ng g〜(-1)(基于50#mu#L的注射量)。在CRM 402提取物中,硒的含量约为1.5#mu#g g〜(-1),相当于材料中硒的总含量约为22%。由于所使用的提取程序,所描述的方法在操作上可以确定。

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