离子交换色谱分离-紫外检测法测定吡啶离子液体阳离子  

Determination of Pyridinium Ionic Liquid Cations by Ion Exchange Chromatography with Ultraviolet Detection

作　　者：刘元昊 孙晓娇[1] 刘峰[1] 于泓[1] 邓春娜 

机构地区：[1]哈尔滨师范大学化学化工学院,哈尔滨150025

出　　处：《中国无机分析化学》2015年第4期83-87,共5页Chinese Journal of Inorganic Analytical Chemistry

基　　金：黑龙江省大学生创新创业训练项目(201410231015;B201307)资助

摘　　要：建立了用离子交换色谱分离-紫外检测法测定N-乙基吡啶、N-丁基吡啶和N-丁基四甲基吡啶3种吡啶离子液体阳离子的方法。采用磺酸型阳离子交换柱,以乙二胺-柠檬酸-乙腈为流动相,研究了流动相和色谱柱温度对离子保留行为的影响和规律。实验发现,吡啶阳离子的保留过程是放热过程。优化后的色谱条件：流动相为乙二胺（0.2 mmol//L）-柠檬酸（0.3 mmol//L）-乙腈（0.5%,v/v,pH=4.2）,流动相流速为1.0mL/min,色谱柱为Shim-pack IC-C1阳离子交换柱,色谱柱温度为30℃。在此条件下3种吡啶阳离子可以达到基线分离。所测阳离子的检出限（S/N=3）分别为0.01、0.01、0.02mg/L,峰面积的相对标准偏差（n=5）小于0.8%。紫外检测法测定化学实验室合成的吡啶离子液体样品,样品加标后测得的加标回收率在96.3%~104%。方法准确、可靠、快速,具有较好的实用价值。A rapid method for simultaneous determination of three pyridinium ionic liquid cations,such as n-erthyl pyridinium cation（[EPy]＋）,n-butyl pyridinium cation（[BPy]＋）and n-hexyl pyridinium cation（[BMPy]＋）by ion exchange chromatography coupled with ultraviolet detection was developed.The effects of mobile phase and column temperature on retention of the cations were investigated with sulfonic acid base cation-exchange column using ethylenediamine-citric acid-acetonitrile as mobile phase.The results indicated that,with the increase of column temperature,the retention times of pyridinium cations were reduced,so the retention process of pyridinium cations is exothermic.The optimum chromatographic conditions were as follows：mobile phase：0.2 mmol/L ethylenediamine-0.3 mmol/L citrate acid-0.5%acetonitrile（pH =4.2）;flow rate：1.0 mL/min;column temperature：30 ℃.Under the optimized conditions,three pyridinium cations were successfully separated.The detection limits（S/N = 3）for[EPy]＋,[BPy]＋,[BMPy]＋were 0.01,0.01 and 0.02 mg/L,respectively.The relative standard deviations（RSDs,n=5）for peak areas were less than 0.8%.The method has been applied to thedetermination of pyridinium ionic liquids synthesized in chemical laboratory with the spiked recoveries of96.3%to 103.7%.The method is accurate,reliable and rapid,and has good practical value.

关 键 词：离子液体 吡啶阳离子 阳离子交换色谱 紫外检测 乙二胺 

分 类 号：O657.32[理学—分析化学] TH744.12[理学—化学]