整体柱和填充柱离子对色谱-间接紫外检测法分析四乙基铵根离子

摘要

Two methods were developed for the determination of tetraethyl ammonium by ion-pair chromatography-indirect ultraviolet detection using a monolithic column and a packed col-umn with ionic liquid as additive in mobile phase. Chromatographic separations were performed on a monolithic column and a packed column both on reversed phase using imidazolium ionic liquid aqueous solution-ion-pair reagent-organic solvent as mobile phase. The effects of the background ultraviolet absorption reagent,detection wavelength,ion-pair reagent,organic sol-vent,column temperature and flow rate on the determination of tetraethyl ammonium were investigated. The difference between the two chromatographic columns was compared and the retention rules were discussed. Under the optimized chromatographic conditions,for tetraethyl ammonium on monolithic column and packed column,the retention times were 2. 40 and 3. 02 min;the detection limits( S/N=3),0. 04 and 0. 07 mg/L;the RSDs( n=5)for peak areas, 0. 16% and 0. 11%;and the RSDs( n=5)for retention times,0. 02% and 0. 01%,respectively. The two methods have been successfully applied to the determination of tetraethyl ammonium ionic liquids synthesized by laboratory. The recoveries of the tetraethyl ammonium after spiking were 98. 2% and 99. 1%,respectively. The two methods can meet the requirements for the quan-titative analysis of tetraethyl ammonium.%建立了整体柱离子对色谱-间接紫外检测和填充柱离子对色谱-间接紫外检测分析四乙基铵根离子的两种方法。用反相整体柱和反相填充柱，以咪唑离子液体-离子对试剂-有机溶剂为流动相，研究了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温和流速对测定四乙基铵根离子的影响，比较了两种色谱柱的差异，并讨论了保留规律。在优化的实验条件下，两种方法测定四乙基铵根离子的保留时间分别是2.40和3.02 min；检出限分别是0.04和0.07 mg／L；峰面积的相对标准偏差分别是0.16％和0.11％；保留时间的相对标准偏差分别是0.02％和0.01％。将这两种方法用于分析实验室合成的溴化四乙基铵离子液体，加标回收率分别为98.2％和99.1％。两种方法均能满足四乙基铵根离子测定的需要。