离子色谱-直接电导检测法分析哌啶离子液体阳离子  

Analysis of piperidinium ionic liquid cations by ion chromatography with direct conductivity detection

作　　者：张仁庆[1] 于泓[1] 刘玉珍[1] 

机构地区：[1]哈尔滨师范大学化学化工学院,黑龙江哈尔滨150025

出　　处：《色谱》2012年第7期728-732,共5页Chinese Journal of Chromatography

基　　金：黑龙江省自然科学基金项目(B200909)

摘　　要：建立了离子色谱-直接电导检测法分析N-甲基,乙基哌啶([MEPi]+)、N-甲基,丙基哌啶([MPPi]+)和N-甲基,丁基哌啶([MBPi]+)3种哌啶离子液体阳离子的方法。采用磺酸型阳离子交换色谱柱,以乙二胺-柠檬酸-乙腈为流动相。考察了流动相组成及色谱柱温度对哌啶阳离子保留的影响,并讨论了保留规律。结果表明,哌啶阳离子的保留是一个放热过程,即哌啶阳离子的保留时间随着色谱柱温度的升高而缩短,且哌啶阳离子同系物的保留符合碳数规律。在以0.2 mmol/L乙二胺-0.3 mmol/L柠檬酸-3%(v/v)乙腈(pH 4.4)为流动相、流速1.0mL/min、柱温30℃条件下,[MEPi]+、[MPPi]+和[MBPi]+3种哌啶阳离子可以在7 min内分离,检出限(信噪比为3)分别为0.14、0.20和0.56 mg/L,峰面积的相对标准偏差(n=5)在1.2%以下。将此方法应用于分析实验室合成的哌啶离子液体样品,加标回收率在97.6%与105.1%之间。本方法准确、可靠、快速,具有较好的实用性。A method of ion chromatography with direct conductivity detection was established to determine three piperidinium ionic liquid cations,i.e.N-methyl,ethyl piperidinium cation（＋）,N-methyl,propyl piperidinium cation（＋） and N-methyl,butyl piperidinium cation（＋）.The effects of eluent types,eluent concentration and column temperature on the retention of the cations were investigated with sulfonic acid base cation exchange column using ethylenediamine-citric acid-acetonitrile as eluent.The results indicated that,with the increase of column temperature,the retention times of piperidinium cations were reduced,so the retention process of piperidinium cations was exothermic.The retentions of piperidinium cation homologue accorded with carbon number rule.The successful separation of the three piperidinium cations within 7 min was achieved using the optimized eluent of 0.2 mmol/L ethylenediamine-0.3 mmol/L citric acid-3% acetonitrile（pH 4.4） at a flow rate of 1.0 mL/min and the column temperature of 30 ℃.Under these conditions,the detection limits at a signal-to-noise ratio of 3 for ＋,＋and ＋were 0.14,0.20 and 0.56 mg/L,respectively.The relative standard deviations（n=5） for peak areas were less than 1.2%.The method has been applied to the determination of piperidinium ionic liquids synthesized in chemical laboratory with the spiked recoveries of 97.6% to 105.1%.The method is accurate,reliable,rapid,and has better practicability.

关 键 词：离子色谱 电导检测 离子液体 哌啶阳离子 

分 类 号：O658[理学—分析化学]