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用于食品样品中铜和镍测定的浊点萃取方法的开发。

Development of a cloud-point extraction method for copper and nickel determination in food samples.

作者信息

Lemos Valfredo Azevedo, Santos Moacy Selis, David Graciete Teixeira, Maciel Mardson Vasconcelos, Bezerra Marcos de Almeida

机构信息

Núcleo de Química Analítica da Bahia (NQA), Laboratório de Química Analítica (LQA), Universidade Estadual do Sudoeste da Bahia, Campus de Jequié, 45206-190 Jequié, BA, Brazil.

出版信息

J Hazard Mater. 2008 Nov 30;159(2-3):245-51. doi: 10.1016/j.jhazmat.2008.02.011. Epub 2008 Feb 14.

Abstract

A new, simple and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of copper and nickel. The metals in the initial aqueous solution were complexed with 2-(2'-benzothiazolylazo)-5-(N,N-diethyl)aminophenol (BDAP) and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified methanol was performed after phase separation, and the copper and nickel contents were measured by flame atomic absorption spectrometry. The variables affecting the cloud-point extraction were optimized using a Box-Behnken design. Under the optimum experimental conditions, enrichment factors of 29 and 25 were achieved for copper and nickel, respectively. The accuracy of the method was evaluated and confirmed by analysis of the followings certified reference materials: Apple Leaves, Spinach Leaves and Tomato Leaves. The limits of detection expressed to solid sample analysis were 0.1 microg g(-1) (Cu) and 0.4 microg g(-1) (Ni). The precision for 10 replicate measurements of 75 microg L(-1) Cu or Ni was 6.4 and 1.0, respectively. The method has been successfully applied to the analysis of food samples.

摘要

已开发出一种新型、简单且通用的浊点萃取(CPE)方法,用于铜和镍的分离与预富集。初始水溶液中的金属与2-(2'-苯并噻唑基偶氮)-5-(N,N-二乙基)氨基酚(BDAP)络合,并加入Triton X-114作为表面活性剂。相分离后,用酸化甲醇稀释富含表面活性剂的相,然后通过火焰原子吸收光谱法测定铜和镍的含量。使用Box-Behnken设计优化了影响浊点萃取的变量。在最佳实验条件下,铜和镍的富集因子分别达到29和25。通过分析以下有证标准物质评估并确认了该方法的准确性:苹果叶、菠菜叶和番茄叶。以固体样品分析表示的检测限为0.1 μg g(-1)(铜)和0.4 μg g(-1)(镍)。对浓度为75 μg L(-1)的铜或镍进行10次重复测量的精密度分别为6.4和1.0。该方法已成功应用于食品样品的分析。

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