离子对色谱-间接紫外检测法分析哌啶离子液体阳离子

摘要

A method was developed for the determination of piperidinium cations by ion-pair chromatography with indirect ultraviolet detection. Chromatographic separation was performed on a reversed-phase C18 column using background ultraviolet absorption reagent-ion-pair rea-gent/organic solvent as mobile phase. The effects of the background ultraviolet absorption rea-gent,detection wavelength,ion-pair reagent,organic solvent,column temperature and flow rate on the determination of piperidinium cations were investigated and the retention rules were studied. The optimized chromatographic conditions for the determination of piperidinium cat-ions were as follows:mobile phase,0. 5 mmol/L 4-aminophenol hydrochloride-0. 1 mmol/L 1-heptanesulfonic acid sodium aqueous solution/methanol(80:20,v/v);detection wavelength, 210 nm;column temperature,30 ℃;flow rate,1. 0 mL/min. Under these conditions,the three piperidinium cations were baseline separated within 4 min. The detection limits( S/N=3)of the piperidinium cations were 0. 137-0. 545 mg/L. The relative standard deviations( n=5)for peak area and retention time were 0. 72% and 0. 37% respectively. The method has been successfully applied to the determination of piperidinium cations in ionic liquids synthesized by chemistry laboratory. The recoveries of piperidinium cations after spiking were 97. 0%-98. 4%. The method is simple,rapid,reproducible,linear,and can meet the quantitative analysis requirement for the determination of piperidinium cations.%建立了快速分析无紫外光吸收的哌啶离子液体阳离子的离子对色谱-间接紫外检测法。采用反相 C18色谱柱，以背景紫外吸收试剂-离子对试剂水溶液/有机溶剂为流动相分离哌啶离子液体阳离子。研究了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温、流速对分离测定哌啶阳离子的影响。最佳色谱条件为：以0.5 mmol/L对氨基苯酚盐酸盐-0.1 mmol/L庚烷磺酸钠水溶液/甲醇（80：20，v/v）为流动相，检测波长210 nm，柱温30℃，流速1.0 mL/min。在此条件下，3种哌啶阳离子可在4 min之内基线分离。所测阳离子的检出限（ S/N=3）为0.137~0.545 mg/L，峰面积和保留时间的相对标准偏差（ n=5）分别不高于0.72％和0.37％。将此方法用于分析实验室合成的哌啶类离子液体，加标回收率为97.0％~98.4％。本方法简便、快速，重现性、线性关系等均能满足哌啶类离子液体阳离子的定量分析要求。