Kandhro Ghulam A, Kazi Tasneem G, Baig Jameel A, Afridi Hassan I, Shah Abdul Q, Sheikh Hafeez R, Kolachi Nida F, Wadhwa Sham K
National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080, Pakistan.
J AOAC Int. 2010 Sep-Oct;93(5):1589-94.
A simple and rapid cloud point extraction method was applied for preconcentration of trace quantities of zinc (Zn) and iron (Fe) in biological samples (serum and urine) of thyroid patients prior to determination by flame atomic absorption spectrometry. The metals in serum and urine samples were complexed with 1-(2-thiazolylazo)-2-naphthol and entrapped in the surfactant octylphenoxypolyethoxyethanol (Triton X-114). After centrifugation, the surfactant-rich phase was diluted with 0.1 M HNO3 in methanol. For optimum recovery of analytes, the influences of the analytical parameters, including pH and amounts of complexing and surfactant reagents, were investigated. Enrichment factors of 66.4 and 70.2 were obtained for the preconcentration of Zn(II) and Fe(III), respectively. The obtained results showed sufficient recoveries (>98%) for Zn(II) and Fe(III) in certified reference materials (CRMs). The proposed method was applied to the determination of Zn(II) and Fe(III) in biological (serum and urine) samples and CRMs.
一种简单快速的浊点萃取方法被应用于甲状腺患者生物样品（血清和尿液）中痕量锌（Zn）和铁（Fe）的预富集，然后通过火焰原子吸收光谱法进行测定。血清和尿液样品中的金属与1-(2-噻唑基偶氮)-2-萘酚络合，并被包埋在表面活性剂辛基苯氧基聚乙氧基乙醇（Triton X-114）中。离心后，富含表面活性剂的相用0.1 M硝酸的甲醇溶液稀释。为了实现分析物的最佳回收率，研究了包括pH值以及络合试剂和表面活性剂试剂用量在内的分析参数的影响。Zn(II)和Fe(III)预富集的富集因子分别为66.4和70.2。所得结果表明，在有证标准物质（CRM）中，Zn(II)和Fe(III)的回收率足够高（>98%）。所提出的方法被应用于生物样品（血清和尿液）以及CRM中Zn(II)和Fe(III)的测定。
