Citak Demirhan, Tuzen Mustafa
Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat, Turkey.
J AOAC Int. 2012 Jul-Aug;95(4):1170-5. doi: 10.5740/jaoacint.11-332.
A cloud point extraction procedure was optimized for the separation and preconcentration of lead(II), cadmium(II), copper(II), and iron(III) ions in various water and canned food samples. The metal ions formed complexes with 2,6-diamino-4-phenyl-1,3,5-triazine that were extracted by surfactant-rich phases in the nonionic surfactant Triton X-114. The surfactant-rich phase was diluted with 1 M HNO3 in methanol prior to its analysis by flame atomic absorption spectrometry. The parameters affecting the extraction efficiency of the proposed method, such as sample pH, complexing agent concentration, surfactant concentration, temperature, and incubation time, were optimized. LOD values based on three times the SD of the blank (3Sb) were 0.38, 0.48, 1.33, and 1.85 microg/L for cadmium(II), copper(II), lead(II), and iron(III) ions, respectively. The precision (RSD) of the method was in the 1.86-3.06% range (n=7). Validation of the procedure was carried out by analysis of National Institute of Standards and Technology Standard Reference Material (NIST-SRM) 1568a Rice Flour and GBW 07605 Tea. The method was applied to water and canned food samples for determination of metal ions.
优化了浊点萃取程序,用于分离和预富集各种水和罐头食品样品中的铅(II)、镉(II)、铜(II)和铁(III)离子。金属离子与2,6-二氨基-4-苯基-1,3,5-三嗪形成配合物,这些配合物在非离子表面活性剂Triton X-114中被富含表面活性剂的相萃取。在通过火焰原子吸收光谱法分析之前,用1 M硝酸甲醇溶液稀释富含表面活性剂的相。对影响该方法萃取效率的参数,如样品pH值、络合剂浓度、表面活性剂浓度、温度和孵育时间进行了优化。基于空白三倍标准偏差(3Sb)的检出限,镉(II)、铜(II)、铅(II)和铁(III)离子分别为0.38、0.48、1.33和1.85 μg/L。该方法的精密度(相对标准偏差,RSD)在1.86 - 3.06%范围内(n = 7)。通过分析国家标准与技术研究院标准参考物质(NIST-SRM)1568a米粉和GBW 07605茶叶对该程序进行了验证。该方法应用于水和罐头食品样品中金属离子的测定。