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聚合离子液体的合成与表征:采用聚合离子液体固相微萃取涂层分析啤酒挥发物。

Analysis of beer volatiles by polymeric imidazolium-solid phase microextraction coatings: Synthesis and characterization of polymeric imidazolium ionic liquids.

机构信息

Department of Physical and Analytical Chemistry, University of Oviedo, Julián Clavería 8, 33006 Oviedo, Spain.

出版信息

J Chromatogr A. 2013 Aug 30;1305:35-40. doi: 10.1016/j.chroma.2013.07.012. Epub 2013 Jul 7.

DOI:10.1016/j.chroma.2013.07.012
PMID:23891206
Abstract

Two polymeric ionic liquids, 3-(but-3″-en-1″-yl)-1-[2'-hydroxycyclohexyl]-1H-imidazol-3-ium bis(trifluoromethanesulfonyl)imide (IL-1) and 1-(2'-hydroxycyclohexyl)-3-(4″-vinylbenzyl)-1H-imidazol-3-ium bis(trifluoromethylsulfonyl)imide (IL-2), have been synthesized by a free radical polymerization reaction and used as coatings for solid-phase microextraction (SPME). These new fibers exhibit good film stability, high thermal stability (270-290°C) and long lifetimes, and are used for the extraction of volatile compounds in lemon beer using gas chromatography separation and flame ionization detection. The scanning electron micrographs of the fiber surface revealed a polymeric ionic liquid (PIL) film, which is distributed homogeneously on the fiber. The developed PIL fiber showed good linearity between 50 and 2000μg/L with regression coefficients in the range of 0.996-0.999. The relative standard deviations (RSD) obtained in the peak area were found to vary between 1% and 12%, which assured that adequate repeatability was achieved. The spiked recoveries for three beer samples ranged from 78.4% to 123.6%. Experimental design has been employed in the optimization of extraction factors and robustness assessment. The polymeric IL-1 butenyl fiber showed a greater efficiency compared to the PDMS-DVB (65μm) and CAR-PDMS (75μm) for the extraction of all of the analytes studied.

摘要

两种聚合离子液体,3-(丁-3”-烯-1”-基)-1-[2'-羟基环己基]-1H-咪唑-3-鎓双(三氟甲磺酰基)亚胺(IL-1)和 1-(2'-羟基环己基)-3-(4”-乙烯基苄基)-1H-咪唑-3-鎓双(三氟甲基磺酰基)亚胺(IL-2),通过自由基聚合反应合成,并用作固相微萃取(SPME)的涂层。这些新纤维表现出良好的膜稳定性、高的热稳定性(270-290°C)和长寿命,并且用于使用气相色谱分离和火焰离子化检测从柠檬啤酒中提取挥发性化合物。纤维表面的扫描电子显微镜照片显示出聚合离子液体(PIL)膜,其均匀分布在纤维上。所开发的 PIL 纤维在 50 至 2000μg/L 之间表现出良好的线性,相关系数在 0.996-0.999 范围内。在峰面积中获得的相对标准偏差(RSD)发现变化在 1%-12%之间,这保证了实现了足够的重现性。三个啤酒样品的加标回收率在 78.4%至 123.6%之间。实验设计已用于优化提取因素和稳健性评估。与 PDMS-DVB(65μm)和 CAR-PDMS(75μm)相比,聚合 IL-1 丁烯基纤维对所有研究的分析物的萃取效率更高。

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