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分光光度法测定硒(IV)的验证:分析应用。

Validation of spectrophotometric method for Se(IV) determination: analytical applications.

机构信息

Faculty of Pharmacy, "Grigore T. Popa" University of Medicine and Pharmacy, Iasi, Romania.

出版信息

Environ Monit Assess. 2014 May;186(5):3277-82. doi: 10.1007/s10661-014-3618-8. Epub 2014 Feb 2.

Abstract

As selenium is an important part of the antioxidant enzymes and also because there are several studies suggesting a possible link between cancer and selenium deficiency, this paper presents a spectrophotometric method for the assay of Se(IV), using N,N-diethyl-p-phenylenediamine monohydrochloride as reagent. The proposed method is based on the reaction between the selenium and potassium iodide in low acidic medium, when iodine is released. This last product will further oxidise the new reagent. The final obtained product is strongly coloured in red and has an absorption maximum at 552 nm and molar extinction coefficient (ε) of 6.1 × 10(4) L mol(-1) cm(-1). The optimum working conditions were established, and the developed method was validated, being characterised by a good linearity (in the range of 0.5-3.0 μg/mL), a limit of detection (0.0573 μg/mL) and a limit of quantification (0.1737 μg/mL). At the same time, the repeatability, the precision of the method and the accuracy were established. The proposed and validated method was applied with good results for the determination of Se(IV) in spring and bottled water from Iasi and also in pharmaceutical and cosmetic products.

摘要

由于硒是抗氧化酶的重要组成部分,并且有几项研究表明癌症与硒缺乏之间可能存在关联,因此本文提出了一种使用 N,N-二乙基对苯二胺单盐酸盐作为试剂测定硒(IV)的分光光度法。该方法基于在低酸性介质中硒与碘化钾之间的反应,释放出碘。该产物将进一步氧化新试剂。最终得到的产物呈强烈的红色,在 552nm 处有最大吸收,摩尔吸光系数(ε)为 6.1×10(4)Lmol(-1)cm(-1)。确定了最佳工作条件,并对所开发的方法进行了验证,该方法具有良好的线性(在 0.5-3.0μg/mL 范围内)、检测限(0.0573μg/mL)和定量限(0.1737μg/mL)。同时,还确定了重复性、方法的精密度和准确性。该方法已成功应用于测定来自雅西的泉水和瓶装水中的硒(IV),以及药物和化妆品中的硒(IV),结果令人满意。

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