Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, P.O. Box 14155-6455, Tehran, Iran.
Food Chem Toxicol. 2011 May;49(5):1086-91. doi: 10.1016/j.fct.2011.01.017. Epub 2011 Jan 25.
In this work, an efficient in situ solvent formation microextraction (ISFME) was combined with stopped-flow injection spectrofluorimetry (SFIS) for the determination of copper. In the proposed approach, thiamine was oxidized with copper(II) to form hydrophobic and highly fluorescent thiochrome (TC), which was subsequently extracted into ionic liquid as an extractant phase. A small amount of an ion-pairing agent (NaPF(6)) was added to the sample solution containing a water-miscible ionic liquid ([Hmim][BF(4)]) to obtain a hydrophobic ionic liquid ([Hmim][PF(6)]), which acted as the extraction phase. After centrifuging, phase separation was performed and the enriched analyte was determined by SFIS. ISFME is an efficient method for separation and preconcentration of metal ions from aqueous solutions with a high ionic strength. Variables affecting the analytical performance were studied and optimized. Under optimum experimental conditions, the proposed method provided a limit of detection (LOD) of 0.024μgL(-1) and a relative standard deviation (RSD) of 2.1%. The accuracy of the combined methodology was evaluated by recovery experiments and by analyzing certified reference material (GBW 07605 Tea). Finally, the proposed method was successfully applied to copper determination in water and food samples.
在这项工作中,高效的原位溶剂形成微萃取(ISFME)与停流注射荧光光谱法(SFIS)相结合,用于测定铜。在所提出的方法中,硫胺素与铜(II)氧化形成疏水性和高荧光性噻嗪(TC),随后将其萃取到离子液体中作为萃取相。在含有水溶性离子液体([Hmim][BF4])的样品溶液中加入少量离子对试剂(NaPF6),以获得疏水性离子液体([Hmim][PF6]),其充当萃取相。离心后,进行相分离,并通过 SFIS 测定富集的分析物。ISFME 是一种从高离子强度水溶液中分离和浓缩金属离子的有效方法。研究并优化了影响分析性能的变量。在最佳实验条件下,所提出的方法提供了 0.024μg L-1 的检测限(LOD)和 2.1%的相对标准偏差(RSD)。通过回收实验和分析认证参考物质(GBW 07605 茶)来评估组合方法的准确性。最后,该方法成功应用于水和食品样品中铜的测定。