摘要
建立了用紫外检测的反相离子对色谱梯度淋洗同时分离测定4种吡啶离子液体阳离子和5种咪唑离子液体阳离子的方法。实验采用ZORBAX Eclipse XDB-C18反相色谱柱,以离子对试剂水溶液(用柠檬酸调节pH值)+乙腈为流动相,考察了离子对试剂种类和浓度、乙腈浓度和色谱柱温度对保留的影响,探讨了相关保留规律,确定最佳色谱条件为:流速1.0 mL/min、柱温30℃,以1.0 mmol/L庚烷磺酸钠水溶液(pH 4.0)-乙腈为淋洗液进行梯度洗脱。在此条件下,4种吡啶阳离子和5种咪唑阳离子在15 min内达到基线分离。检出限(S/N=3)为0.31～0.54 mg/L,峰面积的相对标准偏差为0.10%～0.75%。将该方法用于实验室合成的离子液体样品分析,加标回收率为94%～98%。该方法准确、可靠,具有较好的实用性。
A method was developed for the simultaneous determination of four pyridinium and five imidazolium ionic liquid cations by ion-pair chromatography coupled with ultraviolet detection.Chromatographic separations of the ionic liquid cations were performed on a reversed-phase silica-based column with ion-pair reagent water solution（pH adjusted with citric acid）＋acetonitrile as mobile phase by gradient elution.Effects of ion-pair reagent type,acetonitrile concentration,column temperature and elution gradient on retention factor and separation of the ionic liquid cations were investigated.The retention rules of the ionic liquid cations on the column were discussed.The separation of the four pyridinium and five imidazolium ionic liquid cations were achieved using an optimized elution gradient of 1.0 mmol/L 1-heptanesulfonic acid sodium water solution（pH 4.0,A）＋acetonitrile（B） with a flow rate of 1.0 mL/min at column temperature of 30 ℃.The optimized elution gradient was as follows： 0-3 min,12% B;3-3.5 min,12%-18% B;3.5-6.5 min,18% B;6.5-7.0 min,18%-25% B;7.0-10 min,25% B;10-10.5 min,25%-30% B;10.5-15 min,30% B.Under the optimal conditions,the four pyridinium and five imidazolium ionic liquid cations could be separated in 15 min.Detection limits（S/N=3） were in the range of 0.31-0.54 mg/L.Relative standard deviations（n=5） for the peak areas were 0.10%-0.75%.The method was successfully applied in the determination of the synthesized ionic liquid samples,with spiked recoveries of 94%-98%.The method is accurate,reliable and practical.
出处
《分析测试学报》
CAS
CSCD
北大核心
2012年第2期158-163,共6页
Journal of Instrumental Analysis
基金
黑龙江省自然科学基金项目(B200909)
黑龙江省教育厅科学技术研究项目(11541088)
黑龙江省高校科技创新团队建设计划项目(2011TD010)
关键词
离子对色谱
离子液体
吡啶阳离子
咪唑阳离子
紫外检测
ion-pair chromatography
ionic liquids
pyridinium cations
imidazolium cations
ultraviolet detection
