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使用铱作为永久改性剂并通过原位氧化以实现三甲基硒完全回收,采用石墨炉原子吸收光谱法测定尿液和血清中的总硒。

The determination of total Se in urine and serum by graphite furnace atomic absorption spectrometry using Ir as permanent modifier and in situ oxidation for complete trimethylselenonium recovery.

作者信息

Grinberg Patricia, Gonçalves Rodrigo Araújo, de Campos Reinaldo Calixto

机构信息

Department of Chemistry, Pontifícia Universidade Católica do Rio de Janeiro, Rua Marquês de São Vicente, 225, Rio de Janeiro, 22453-900, Brazil.

出版信息

Anal Bioanal Chem. 2005 Dec;383(7-8):1044-51. doi: 10.1007/s00216-005-0014-9. Epub 2005 Nov 3.

Abstract

The present work evaluated the use of iridium (Ir) as permanent modifier for the determination of total selenium in urine and serum by graphite furnace atomic absorption spectrometry. Concerning urine, the presence of trimethylselenonium (TMSe(+)) was especially considered. Pyrolysis and atomization temperatures of 1,000 and 2,100 degrees C, respectively, were used. For nondigested urine and serum samples, 0.2% v/v HNO(3) and Triton X-100 were used as diluents, respectively, and the same initial platform Ir treatment was effective for up to 1,100 atomization cycles. Good precision [less than 5% relative standard deviation (RSD)] can be achieved with the proposed method. Low TMSe(+) recovery was observed for nondigested urine samples. Thus, if this species is to be considered in urine analysis, a previous external mineralization step was found to be necessary. Alternatively, an in situ oxidation treatment was developed. Detection limits of 8, 10, and 7 mug l(-1) were obtained after dilution, microwave-assisted digestion, and in situ oxidation procedures, respectively. The accuracy of the method was validated by the analysis of certified reference or commercial quality control materials and spiked samples.

摘要

本研究评估了铱(Ir)作为石墨炉原子吸收光谱法测定尿液和血清中总硒的永久性改性剂的应用。对于尿液,特别考虑了三甲基硒鎓(TMSe(+))的存在。分别使用1000℃和2100℃的热解温度和原子化温度。对于未消化的尿液和血清样品,分别使用0.2% v/v HNO(3)和Triton X-100作为稀释剂,相同的初始平台Ir处理对于多达1100个原子化循环都是有效的。所提出的方法可实现良好的精密度[相对标准偏差(RSD)小于5%]。未消化的尿液样品中观察到TMSe(+)回收率较低。因此,如果在尿液分析中要考虑这种物质,发现有必要进行先前的外部矿化步骤。或者,开发了一种原位氧化处理方法。经过稀释、微波辅助消解和原位氧化程序后,检测限分别为8、10和7 μg l(-1)。通过分析有证标准物质或商业质量控制物质以及加标样品验证了该方法的准确性。

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