Abstract: A novel allyl trifluoromethanesulfonimide （allyl Ntf） cation exchanger was synthesized. The allyl Ntf （192 mg） was taken and dissolved in 10.0 mL of acetonitrile solution containing 0.01 mol·L⁻¹ tetra-n-butylammonium phosphate, the mixture was used as the electrolyte solution. Using the electropolymerization method, the allyl Ntf was modified on the surface of the pretreated glassy carbon electrode （GCE）, thus the allyl Ntf-GCE was constructed. Combined with ion chromatography, the contents of methylamine, ethylamine and propylamine in the filtered samples were simultaneously determined. As shown by the results, linear relationships between the corresponding peak height and the concentration of methylamine, ethylamine, and propylamine were found in definite ranges, with detection limits in the range of 7.6×10⁻⁷‒9.3×10⁻⁶ mol·L⁻¹. Test for recovery was made by the standard addition method on actual sample, giving results in the range of 95.2%−98.9%, and RSDs （n=5） of the determined values were in the range of 2.3%−2.9%. The method was applied to the analysis of river water sample, the absolute values of relative deviations between the detection results and those obtained by the ion chromatography conductivity detector were less than 10%. Further, using aniline as the functional monomer and trimethylamine （TMA） as the template molecule, a molecularly imprinted polymer （MIP） film with specific recognition for TMA was constructed on the surface of the allyl Ntf-GCE, forming the TMA-MIP electrode. The contents of TMA in filtered samples were determined by electrochemical method. As shown by the results, linear relationship between the corresponding potential value and the concentration of TMA was in the range of 0.01‒1.00 μmol·L⁻¹, with detection limit of 3 nmol·L⁻¹. This method was applied to the analysis of 3 human urine samples, the detected amounts of TMA were in the range of 0.163‒0.197 μmol·L⁻¹.