色谱

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梯度淋洗离子对色谱法测定咪唑离子液体中的阳离子

高微, 于泓*, 马亚杰   

  1. 哈尔滨师范大学化学化工学院, 黑龙江 哈尔滨 150025
  • 收稿日期:2009-12-19 修回日期:2010-02-19 出版日期:2010-06-28 发布日期:1980-06-25
  • 通讯作者: 于泓

Determination of imidazolium ionic liquid cations by ion-pair chromatography using gradient elution

GAO Wei, YU Hong*, MA Yajie   

  1. College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China
  • Received:2009-12-19 Revised:2010-02-19 Online:2010-06-28 Published:1980-06-25
  • Contact: YU Hong

摘要: 采用梯度淋洗离子对色谱-紫外检测(IPC-UV)法分离测定5种咪唑离子液体中的阳离子。实验采用ZORBAX Eclipse XDB C18色谱柱,以离子对试剂与乙腈为流动相,首先考察了离子对试剂种类和浓度、乙腈浓度和色谱柱温度对咪唑阳离子保留的影响,然后确定了最适宜分离的色谱条件。在此条件下可同时基线分离5种咪唑阳离子。所测阳离子的检出限(S/N=3)为0.05~0.30 mg/L,峰面积的相对标准偏差(RSD, n=5)在0.1%以下。将此方法用于分析实验室合成的2种1-烷基-3-甲基咪唑离子液体中的阳离子,加标回收率在98.6%~102.1%之间。本方法准确、可靠,具有较好的实用性。

关键词: 离子对色谱, 离子液体 , 梯度淋洗, 紫外检测

Abstract: Determination of five imidazolium ionic liquid cations by ion-pair chromatography was carried out using ultraviolet-visible spectrophotometry (UV/VIS)detection. Chromatographic separations were performed on a ZORBAX Eclipse XDB-C18 column with 1-heptanesulfonic acid sodium (adjusted by citric acid to pH 4.0)+acetonitrile as eluent. The effects of ion-pair reagents, acetonitrile concentration and column temperature on retention of the cations were investigated. The retention factor of imidazolium cation on column was increased with the increase of the concentration of 1-heptanesulfonic acid sodium. With the increase of the concentration of acetonitrile, the retention time of imidazolium cation was obviously shortened and the peak shape was improved. Under the optimum conditions, detection limits (S/N=3) for the cations were 0.05-0.30 mg/L. Relative standard deviations (RSDs) for peak areas were less than 0.1%. The method has been successfully applied to the determination of two ionic liquids by chemically synthesized in laboratory with the recoveries of the cations of 98.6%-102.1% after spiking.

Key words: gradient elution, ionic liquids , ultraviolet detection, ion-pair chromatography