Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, Tabriz, Iran.
J Chromatogr A. 2015 Jan 30;1379:24-33. doi: 10.1016/j.chroma.2014.12.049. Epub 2014 Dec 24.
In this study, for the first time, a dispersive liquid-liquid microextraction technique using a ternary solvent mixture is reported. In order to extract five phthalate esters and di(2-ethylhexyl) adipate with different polarities from aqueous samples, a simplex centroid experimental design method was used to select an optimal mixture of ternary solvents prior to gas chromatographyflame ionization detection. In this work, dimethyl formamide as a disperser solvent containing dichloromethane, chloroform, and carbon tetrachloride as a ternary extraction solvent mixture is injected into sample solution and a cloudy solution is formed. After centrifuging, 250μL of the obtained sedimented phase was transferred into another tube and 5μL DMF was added to it. Then, the tube was heated in a water bath at 75°C for 5min in order to evaporate the main portion of the extraction solvents. Finally, 2μL of the remained phase is injected into the separation system. Under the optimum extraction conditions, the method shows wide linear ranges and low limits of detection and quantification between 0.03-0.15 and 0.09-0.55μgL(-1), respectively. Enrichment factors and extraction recoveries are in the ranges of 980-4500 and 20-90%, respectively. The method is successfully applied in the determination of the target analytes in mineral water, soda, lemon juice, vinegar, dough, and yogurt packed in plastic packages.
在本研究中,首次报道了一种使用三元溶剂混合物的分散液液微萃取技术。为了从水样中提取具有不同极性的五种邻苯二甲酸酯和己二酸二(2-乙基己基)酯,采用单纯形质心法实验设计方法,在气相色谱-火焰离子化检测之前选择最佳的三元溶剂混合物。在这项工作中,二甲基甲酰胺作为分散溶剂,含有二氯甲烷、三氯甲烷和四氯化碳作为三元萃取溶剂混合物,注入样品溶液中,形成浑浊溶液。离心后,将 250μL 所得沉淀相转移至另一管中,并加入 5μL DMF。然后,将管在 75°C 的水浴中加热 5min,以蒸发大部分萃取溶剂。最后,将 2μL 剩余相注入分离系统。在最佳萃取条件下,该方法的线性范围较宽,检测限和定量限分别在 0.03-0.15 和 0.09-0.55μgL(-1)之间。富集因子和萃取回收率分别在 980-4500 和 20-90%之间。该方法成功应用于测定塑料包装的矿泉水、苏打水、柠檬汁、醋、面团和酸奶中的目标分析物。