Department of Analytical Chemistry, University of P.J. Safárik, SK-04154 Kosice, Slovak Republic.
Talanta. 2010 Oct 15;82(5):1958-64. doi: 10.1016/j.talanta.2010.08.028. Epub 2010 Aug 21.
This paper presents a novel approach to dispersive liquid-liquid microextraction (DLLME), based on the use of an auxiliary solvent for the adjustment of density. The procedure utilises a solvent system consisting of a dispersive solvent, an extraction solvent and an auxiliary solvent, which allows for the use of solvents having a density lower than that of water as an extraction solvent while preserving simple phase separation by centrifugation. The suggested approach could be an alternative to procedures described in the literature in recent months and which have been devoted to solving the same problem. The efficiency of the suggested approach is demonstrated through the determination of gold based on the formation of the ion pair Au(CN)(2) anion with Astra Phloxine (R) reagent and its extraction using the DLLME procedure with subsequent UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric detection. The optimum conditions were found to be: pH 3; 0.8 mmol L(-1) K(4)[Fe(CN)(6)]; 0.12 mmol L(-1) R; dispersive solvent, methanol; extraction solvent, toluene; auxiliary solvent, tetrachloromethane. The calibration plots were linear in the ranges 0.39-4.7 mg L(-1) and 0.5-39.4 μg L(-1) for UV-VIS and GFAAS detection, respectively; thus enables the application of the developed method in two ranges differing from one from another by three orders of magnitude. The presented approach can be applied to the development of DLLME procedures for the determination of other compounds extractable by organic solvents with a density lower than that of water.
本文提出了一种基于辅助溶剂调整密度的分散液液微萃取(DLLME)新方法。该方法采用分散溶剂、萃取溶剂和辅助溶剂组成的溶剂体系,允许使用密度低于水的溶剂作为萃取溶剂,同时通过离心实现简单的相分离。该方法可以替代最近几个月文献中描述的、用于解决相同问题的程序。通过用 Astra Phloxine(R)试剂与金形成离子对Au(CN)(2)阴离子,并采用 DLLME 程序萃取,随后进行 UV-VIS 分光光度法和石墨炉原子吸收光谱法检测,证明了所提出方法的效率。最佳条件为:pH 3;0.8 mmol L(-1) K(4)[Fe(CN)(6)];0.12 mmol L(-1) R;分散溶剂为甲醇;萃取溶剂为甲苯;辅助溶剂为四氯化碳。对于 UV-VIS 和 GFAAS 检测,校准曲线分别在 0.39-4.7 mg L(-1)和 0.5-39.4 μg L(-1)范围内呈线性;从而使开发的方法能够在两个相差三个数量级的范围内应用。该方法可应用于开发其他可被有机溶剂萃取、密度低于水的化合物的 DLLME 程序。