Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.
Talanta. 2012 Sep 15;99:1004-10. doi: 10.1016/j.talanta.2012.07.089. Epub 2012 Aug 7.
A new method based on simultaneous derivatization and dispersive liquid-liquid microextraction in one step is developed for determination of five anilines in different aqueous samples. In this method, acetonitrile containing microlitre-level of butylchloroformate was rapidly injected into aqueous sample by a syringe. After centrifugation of the cloudy solution, the fine droplets of the butylchloroformate containing the derivatized analytes were sedimented in the bottom of the conical test tube. Then, 0.5 μL of the settled phase was injected into gas chromatography-flame ionization detector. Under optimum conditions the enrichment factors, extraction recoveries and enhancement factors were high and ranged between 197 and 298, 47 and 69%, and 4.7 and 6.2, respectively. Linearity was observed in the range of 10-10,000 μg L(-1) (except for 4-chloroaniline), and the relative standard deviations (RSD %) were lower than 5.2% (n=6). The limits of detection of the six anilines ranged from 1 to 3 μg L(-1). Different aqueous samples including tap, river and well waters as well as wastewaters were successfully analyzed. In this method the extraction solvent and derivatization agent are the same and the derivatization reaction was carried out under mild conditions. This method has several advantages over other reported techniques, being very simple, rapid and less hazardous for the environment.
基于同时衍生化和分散液液微萃取的一步新方法被开发用于测定不同水样中的五种苯胺。在该方法中，含微量丁基氯甲酸酯的乙腈通过注射器迅速注入水样中。将混浊溶液离心后，含衍生化分析物的丁基氯甲酸酯的细小液滴沉淀在锥形试管的底部。然后，将 0.5 μL 的沉降相注入气相色谱-火焰离子化检测器。在最佳条件下，富集因子、萃取回收率和增强因子较高，范围在 197 到 298、47 到 69%和 4.7 到 6.2 之间。在 10-10000 μg L(-1)（除 4-氯苯胺外）范围内观察到线性，相对标准偏差（RSD%）低于 5.2%（n=6）。六种苯胺的检测限范围为 1 到 3 μg L(-1)。成功分析了不同的水样，包括自来水、河水和井水以及废水。在该方法中，萃取溶剂和衍生化剂是相同的，并且衍生化反应在温和条件下进行。与其他报道的技术相比，该方法具有几个优点，即非常简单、快速且对环境危害较小。
