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两步堆积法:扫集和胶束增溶-溶剂堆积法,使用长链阳离子离子液体表面活性剂。

Two-step stacking by sweeping and micelle to solvent stacking using a long-chain cationic ionic liquid surfactant.

机构信息

Key Laboratory of Chemistry of Northwestern Plant Resources, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, PR China.

出版信息

J Sep Sci. 2012 Feb;35(4):589-95. doi: 10.1002/jssc.201100759.

DOI:10.1002/jssc.201100759
PMID:22389909
Abstract

Coupling of long-chain ionic liquid (LCIL)-based sweeping and micelle to solvent stacking (MSS) in CZE for anionic compounds was proposed. N-Cetyl-N-methylpyrrolidinium bromide (C16MPYBr) was used as a novel cationic surfactant. The capillary column was conditioned with poly(1-vinyl-3-butylimidazolium) bromide, a kind of polymeric ionic liquid, to obtain the anodic electroosmotic flow (EOF). There is a micellar solution (MS) zone which is prepared with C16MPYBr before the sample zone. The micelles penetrated into the sample zone, swept and transported the analytes toward the micelle to solvent boundary (MSSB). Meanwhile, a sufficient amount of methanol in the background solution (BGS) resulted in the reversal of effective electrophoretic mobility of analytes and completed the MSS. Under optimal conditions, good linearity (0.9988–0.9999) was obtained for model analytes in a wide linear range with limits of detection (LODs) from 0.025 to 0.25 mg/L. The intraday and interday repeatabilities (%RSD, n=5, 10) were acceptable in the range from 2.12 to 7.29%. 34 and 25 times increases in peak area sensitivity for benzoic acid (BA) and 2-nitrophenol (2-NP) and 60 times increase in peak height sensitivity for 4-chlorophenol (4-CP) were obtained. The proposed method is applied to analyze two spiked environmental water samples obtaining satisfactory recoveries.

摘要

本文提出了一种在 CZE 中,将基于长链离子液体(LCIL)的胶束扫除与溶剂堆积(MSS)相耦合,用于分离阴离子化合物的方法。采用新型阳离子表面活性剂 N-十六烷基-N-甲基吡咯烷溴化物(C16MPYBr)。毛细管柱经聚(1-乙烯基-3-丁基咪唑溴化物)预处理,获得阳极电渗流(EOF)。在样品区之前,存在一个胶束溶液(MS)区,由 C16MPYBr 组成。胶束渗透到样品区,扫除并将分析物朝着胶束-溶剂边界(MSSB)迁移。同时,背景溶液(BGS)中甲醇的大量存在导致分析物有效电泳迁移率发生反转,完成了 MSS。在最佳条件下,模型分析物在较宽的线性范围内(线性范围为 0.9988-0.9999)获得了良好的线性关系,检出限(LOD)范围为 0.025-0.25mg/L。日内和日间重复性(%RSD,n=5,10)在 2.12-7.29%范围内是可以接受的。苯甲酸(BA)和 2-硝基苯酚(2-NP)的峰面积灵敏度分别提高了 34 倍和 25 倍,4-氯苯酚(4-CP)的峰高灵敏度提高了 60 倍。该方法已成功应用于分析两种加标环境水样,获得了令人满意的回收率。

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