Suárez Ruth, Clavijo Sabrina, Avivar Jessica, Cerdà Víctor
Laboratory of Environmental Analytical Chemistry - LQA2, University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca, Spain.
Laboratory of Environmental Analytical Chemistry - LQA2, University of the Balearic Islands, Cra. Valldemossa km 7.5, 07122 Palma de Mallorca, Spain.
Talanta. 2016 Feb 1;148:589-95. doi: 10.1016/j.talanta.2015.10.031. Epub 2015 Oct 23.
An environmental friendly and fully automated method using in-syringe magnetic stirring assisted dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography has been developed for the determination of UV filters in environmental water samples. The main "green" features on this method are the use of an ionic liquid as extracting solvent, avoiding the use of chlorinated solvents, and the on-line microextraction, preconcentration, separation and detection minimizing the use of reagents and so the waste generation. After sample treatment, 20 µL of the organic droplet was injected onto the HPLC-UV system. Various parameters affecting the extraction efficiency were studied using multivariate optimization approach, including the quantity of extraction and dispersive solvents, extraction and sedimentation time, ionic strength and pH. Under optimized conditions, limits of detection were within the range of 0.08-12 µg/L, for 3.5 mL sample volume. Linearity ranges were up to 500 µg/L for the UV-filters studied. Furthermore, enrichment factors ranging from 11 to 23 folds were obtained. Intra- and inter-assay precisions were 6% and 8%, respectively. Finally, the proposed method was successfully applied to determine UV filters in surface seawater and swimming pool samples attaining satisfactory recoveries over the range of 89-114% and 86-107%, respectively.
已开发出一种环境友好且全自动的方法,即采用注射器内磁搅拌辅助分散液液微萃取结合高效液相色谱法来测定环境水样中的紫外线过滤剂。该方法的主要“绿色”特性包括使用离子液体作为萃取溶剂,避免使用氯化溶剂,以及在线微萃取、预浓缩、分离和检测,从而最大限度地减少试剂使用及废物产生。样品处理后,将20 μL有机液滴注入高效液相色谱 - 紫外系统。采用多变量优化方法研究了影响萃取效率的各种参数,包括萃取溶剂和分散溶剂的用量、萃取和沉降时间、离子强度及pH值。在优化条件下,对于3.5 mL样品体积,检测限在0.08 - 12 μg/L范围内。所研究的紫外线过滤剂的线性范围高达500 μg/L。此外,富集倍数在11至23倍之间。批内和批间精密度分别为6%和8%。最后,该方法成功应用于测定地表海水和游泳池水样中的紫外线过滤剂,回收率分别在89 - 114%和86 - 107%范围内,结果令人满意。