整体柱反相液相色谱-间接紫外检测法分析四丙基铵根

Determination of tetrapropyl ammonium by reversed-phase liquid chromatography-indirect ultraviolet detection using a monolithic column

建立了一种反相液相色谱-间接紫外检测分离无紫外光吸收的四丙基铵根离子(TPA)方法。选用反相硅胶整体柱,咪唑类离子液体水溶液/有机溶剂作为淋洗液,研究了背景紫外吸收剂、色谱柱、淋洗液、流速及柱温对分析TPA的影响,并讨论了保留规律。设定检测波长210 nm,柱温30℃,流速1.0 mL/min,0.7 mmol/L[EM IM][BF4]水溶液(通过乙酸调节pH 4.5)/甲醇(80/20,V/V)作为淋洗液,TPA的保留时间2.11 min,检出限0.78 mg/L,峰面积的相对标准偏差(RSD)0.70%,保留时间的RSD为0.030%。方法用于检测实验室合成的溴化四丙基铵离子液体样品,加标回收率99.2%。

A reversed-phase liquid chromatography-indirect ultraviolet detection method was developed for the determination of tetrapropyl ammionium （TPA） that have no ultraviolet absorption. The reversed phase silica gel monolithic column and eluent of imidazolium ionic liquid aqueous solution/ organic solvent were used. The effects of background UV absorber, column, eluent, flow rate and column temperature on the determination of TPA were investigated and the retention rules were discussed. The instrumental parameters were set as follows： detection wavelength： 210 nm, column temperature ： 30℃, flow rate ： 1 mL/min. 0.7 mmoL/L 1-ethyl-3-methylimidazolium tetrafluoroborate solution （pH 4. 5 adjusted by acetic acid）/methanol （80/20, V/V） was used as eluent. The retention time of TPA was 2.11 min, with the detection limit of 0.78 mg/L, and the relative standard deviation （RSD） of peak area and retention time were 0. 70% and 0. 030% , respectively. In this way, laboratory synthetic ion liquid samples of four propyl ammonium bromide were determined with a recovery rate of 99.2%. This method is efficient and practical.