Department of Analytical Chemistry, Faculty of Chemistry, University of Mazandaran, Babolsar, Iran.
Talanta. 2012 Oct 15;100:447-53. doi: 10.1016/j.talanta.2012.08.019. Epub 2012 Aug 23.
A simple, fast and efficient method for the preconcentration of phthalate esters (PEs) in water samples was developed using magnetic stirring-assisted dispersive liquid-liquid microextraction (MSA-DLLME) followed by high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). This novel microextraction method is based on the fast injection of extracting solvent into the aqueous solution, which is being stirred by a magnetic stirrer, to form a cloudy binary component solvent (aqueous solution:extracting solvent) system. The extraction parameters such as type and volume of extracting solvent, pH of sample, salt addition, extraction time and stirring rate were optimized. Under the optimal conditions (extracting solvent: 200 μL dodecane; pH of sample: 6.5; extraction time: 5 min; stirring rate: 1000 rpm), linearity was observed in the range of 2-1000 μg L(-1) for dimethyl phthalate (DMP) and 1-1000 μg L(-1) for diethyl phthalate (DEP), benzyl butyl phthalate (BBP) and di-n-butyl phthalate (DBP) with correlation determination values above 0.99 for them. The limits of detection and quantification were ranged from 0.13 to 0.38 μg mL(-1) and 0.43 to 1.27 μg mL(-1), respectively. The ranges of intra-day and inter-day precisions (n=5) at 100 μg L(-1) of PEs were 1.50-2.65% and 2.31-3.35%, respectively. Finally, the MSA-DLLME method was successfully applied for preconcentration of PEs in drinking and environmental water samples.
一种简单、快速、高效的水样中邻苯二甲酸酯（PEs）浓缩方法，采用磁搅拌辅助分散液液微萃取（MSA-DLLME）结合高效液相色谱-紫外检测（HPLC-UV）。这种新型微萃取方法基于将萃取溶剂快速注入正在搅拌的水溶液中，形成混浊的二元溶剂（水相：萃取溶剂）体系。优化了萃取参数，如萃取溶剂的类型和体积、样品 pH 值、加盐、萃取时间和搅拌速度。在最佳条件下（萃取溶剂：200 μL 正十二烷；样品 pH 值：6.5；萃取时间：5 min；搅拌速度：1000 rpm），二甲基邻苯二甲酸酯（DMP）的线性范围为 2-1000 μg L(-1)，二乙基邻苯二甲酸酯（DEP）、邻苯二甲酸苄丁酯（BBP）和邻苯二甲酸二正丁酯（DBP）的线性范围为 1-1000 μg L(-1)，相关系数均大于 0.99。检测限和定量限范围分别为 0.13-0.38 μg mL(-1)和 0.43-1.27 μg mL(-1)。在 100 μg L(-1)的 PEs 浓度下，日内和日间精密度（n=5）的范围分别为 1.50-2.65%和 2.31-3.35%。最后，该方法成功应用于饮用水和环境水样中 PEs 的预浓缩。
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