Wang Miaoyu, Yu Hong, Li Ping, Li Jie, Gao Yufeng
Se Pu. 2014 Jul;32(7):773-8. doi: 10.3724/sp.j.1123.2014.03036.
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 reagent/organic solvent as mobile phase. The effects of the background ultraviolet absorption reagent, 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 cations 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 degrees C; 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.
建立了一种采用离子对色谱-间接紫外检测法测定哌啶阳离子的方法。采用反相C18色谱柱，以具有背景紫外吸收的试剂-离子对试剂/有机溶剂为流动相进行色谱分离。考察了背景紫外吸收试剂、检测波长、离子对试剂、有机溶剂、柱温及流速对哌啶阳离子测定的影响，并研究了保留规律。测定哌啶阳离子的优化色谱条件如下：流动相为0.5 mmol/L盐酸4-氨基苯酚-0.1 mmol/L庚烷磺酸钠水溶液/甲醇（80:20，v/v）；检测波长为210 nm；柱温为30℃；流速为1.0 mL/min。在此条件下，3种哌啶阳离子在4 min内实现基线分离。哌啶阳离子的检测限（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）分别为0.72%和0.37%。该方法已成功应用于化学实验室合成的离子液体中哌啶阳离子的测定。加标后哌啶阳离子的回收率为97.0%～98.4%。该方法简便、快速、重现性好、线性关系良好，能够满足哌啶阳离子测定的定量分析要求。
