Chinese Journal of Chromatography ›› 2013, Vol. 31 ›› Issue (10): 969-973.DOI: 10.3724/SP.J.1123.2013.03010

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Rapid determination of N-methyl,propyl-morpholinium cation by ion-pair chromatography on monolithic column with indirect ultraviolet detection

SUN Yimeng, YU Hong   

  1. College of Chemistry and Chemical Engineering, Harbin Normal University, Harbin 150025, China
  • Received:2013-03-04 Revised:2013-03-29 Online:2013-10-28 Published:2013-10-08

Abstract:

A fast analytical method was developed for the determination of N-methyl,propyl-morpholinium cation (MPMo) without UV absorption group by ion-pair chromatography-indirect UV detection. Chromatographic separation was performed on a reversed-phase silica-based monolithic column using background UV absorption reagent aqueous solution-ion-pair reagent aqueous solution-organic solvent as the mobile phase. The effects of the background UV absorption reagent, detection wavelength, ion-pair reagent, organic solvent, column temperature and flow rate on the determination of MPMo were investigated. It was found that the morpholinium cation could be determined well with (0.5 mmol/L 4-aminophenol hydrochloride-0.1 mmol/L 1-heptanesulfonic sodium) aqueous solution-methanol (9:1, v/v) as mobile phase at the UV detection wavelength of 230 nm, the column temperature of 30 ℃ and the flow rate of 1.0 mL/min. Under these conditions, the retention time of MPMo was 2.966 min. The limit of detection for MPMo was 0.07 mg/L (S/N=3). The relative standard deviations (n=5) for the peak area and retention time were 2.1% and 0.02%, respectively. The method was successfully applied to the determination of morpholinium ionic liquid synthesized by a chemistry laboratory. Recovery of MPMo after spiking was 98.8%. The results showed that this method is simple and rapid.

Key words: 4-aminophenol hydrochloride, indirect ultraviolet detection, ionic liquid, ion-pair chromatography, monolithic column, morpholinium cation

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