Department of Chemistry, National University of Singapore, Singapore, Singapore.
J Chromatogr A. 2011 Jul 15;1218(28):4299-306. doi: 10.1016/j.chroma.2011.05.031. Epub 2011 May 14.
For the first time, an ionic liquid based three-phase liquid-liquid-liquid solvent bar microextraction (IL-LLL-SBME) was developed for the analysis of phenols in seawater samples. The ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM][PF(6)]), was used as the intermediary solvent for LLL-SBME, enhancing the extraction efficiency for polar analytes. In the procedure, the analytes were extracted from the aqueous sample into the ionic liquid intermediary and finally, back-extracted into an aqueous acceptor solution in the lumen of the hollow fiber. The porous polypropylene membrane acted as a filter to prevent potential interfering materials from being extracted, and no additional cleanup was required. After extraction, the acceptor solution could be directly injected into a high-performance liquid chromatographic system for analysis. Six phenols, 2-nitrophenol, 4-chlorophenol, 2,3-dichlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol were selected here as model compounds for developing and evaluating the method. The most influential extraction parameters were evaluated, including the ionic liquid, the composition of donor solution and acceptor solution, the extraction time and the extraction temperature, the effect of ionic strength, and the agitation speed. Under the most favorable extraction parameters, the method showed good linearity (from 0.05-50 to 0.5-50 μg/L, depending on the analytes) and repeatability of extractions (RSD below 8.3%, n=5). The proposed method was compared to conventional three-phase LLL-SBME and ionic liquid supported hollow fiber protected three-phase liquid-liquid-liquid microextraction, and showed higher extraction efficiency. The proposed method was demonstrated to be a simple, fast, and efficient method for the analysis of phenols from environmental water samples.
首次开发了基于离子液体的三相液-液-液溶剂微萃取(IL-LLL-SBME),用于海水样品中酚类物质的分析。离子液体 1-丁基-3-甲基咪唑六氟磷酸盐([BMIM][PF(6)])被用作 LLL-SBME 的中间溶剂,增强了对极性分析物的萃取效率。在该过程中,分析物从水相样品中被萃取到离子液体中间相,最终被反萃取到中空纤维内腔中的水接受相中。多孔聚丙烯膜作为过滤器,防止潜在的干扰物质被萃取,无需进行额外的净化。萃取后,接受溶液可直接注入高效液相色谱系统进行分析。选择六种酚类物质,包括 2-硝基苯酚、4-氯苯酚、2,3-二氯苯酚、2,4-二氯苯酚、2,4,6-三氯苯酚和五氯苯酚,作为开发和评估方法的模型化合物。评估了最具影响力的萃取参数,包括离子液体、供体溶液和接受溶液的组成、萃取时间和萃取温度、离子强度的影响以及搅拌速度。在最有利的萃取参数下,该方法显示出良好的线性范围(取决于分析物,从 0.05-50 至 0.5-50μg/L)和萃取重复性(RSD 低于 8.3%,n=5)。与传统三相 LLL-SBME 和离子液体支撑的中空纤维保护三相液-液-液微萃取相比,该方法显示出更高的萃取效率。该方法被证明是一种简单、快速、高效的方法,用于分析环境水样中的酚类物质。