Sarafraz-Yazdi A, Mofazzeli F, Es'haghi Z
Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Iran.
Talanta. 2009 Jul 15;79(2):472-8. doi: 10.1016/j.talanta.2009.04.015. Epub 2009 Apr 16.
A new and fast hollow fiber based liquid phase microextraction (HF-LPME) method using volatile organic solvents coupled with high-performance liquid chromatography (HPLC) was developed for determination of aromatic amines in the environmental water samples. Analytes including 3-nitroaniline, 3-chloroaniline and 4-bromoaniline were extracted from 6 mL basic aqueous sample solution (donor phase, NaOH 1 mol L(-1)) into the thin film of organic solvent that surrounded and impregnated the pores of the polypropylene hollow fiber wall (toluene, 20 microL), then back-extracted into the 6 mL acidified aqueous solution (acceptor phase, HCl 0.5 mol L(-1)) in the lumen of the two-end sealed hollow fiber. After the extraction, 5 microL of the acceptor phase was withdrawn into the syringe and injected directly into the HPLC system for the analysis. The parameters influencing the extraction efficiency including the kind of organic solvent and its volume, composition of donor and acceptor phases and the volume ratio between them, extraction time, stirring rate, salt addition and the effect of the analyte complexation with 18-crown-6 ether were investigated and optimized. Under the optimal conditions (donor phase: 6 mL of 1 mol L(-1) NaOH with 10% NaCl; organic phase: 20 microL of toluene; acceptor phase: 6 microL of 0.5 mol L(-1) HCl and 600 mmol L(-1) 18-crown-6 ether; pre-extraction and back-extraction times: 75 s and 10 min, respectively; stirring rate: 800 rpm), the obtained EFs were between 259 and 674, dynamic linear ranges were 0.1-1000 microg L(-1) (R>0.9991), and also the limits of detection were in the range of 0.01-0.1 micro gL(-1). The proposed procedure worked very well for real environmental water samples with microgram per liter level of the analytes, and good relative recoveries (91-102%) were obtained for the spiked sample solutions.
开发了一种基于中空纤维的新型快速液相微萃取（HF-LPME）方法，该方法使用挥发性有机溶剂并结合高效液相色谱（HPLC）来测定环境水样中的芳香胺。分析物包括3-硝基苯胺、3-氯苯胺和4-溴苯胺，它们从6 mL碱性水样溶液（供体相，1 mol L(-1) NaOH）中被萃取到围绕并浸渍聚丙烯中空纤维壁孔隙的有机溶剂薄膜（20 μL甲苯）中，然后再反萃取到两端密封的中空纤维内腔中的6 mL酸化水溶液（受体相，0.5 mol L(-1) HCl）中。萃取后，取5 μL受体相注入注射器，直接进样到HPLC系统进行分析。研究并优化了影响萃取效率的参数，包括有机溶剂的种类及其体积、供体相和受体相的组成及其体积比、萃取时间、搅拌速率、加盐情况以及分析物与18-冠-6醚络合的影响。在最佳条件下（供体相：6 mL含10% NaCl的1 mol L(-1) NaOH；有机相：20 μL甲苯；受体相：6 μL含600 mmol L(-1) 18-冠-6醚的0.5 mol L(-1) HCl；预萃取和反萃取时间分别为75 s和10 min；搅拌速率：800 rpm），得到的萃取因子在259至674之间，动态线性范围为0.1 - 1000 μg L(-1)（R > 0.9991），检测限在0.01 - 0.1 μg L(-1)范围内。所提出的方法对于每升含微克级分析物的实际环境水样效果良好，加标样品溶液的相对回收率良好（91 - 102%）。
