A rapid, convenient and precise chromatographic method for the simultaneous determination of chlorpheniramine and maleate is described. By the use of a Capcell Pak C 8 column and an isocratic mobile phase containing 50 mM KH 2 PO 4 , 5 mM tetra-n-butylammonium phosphate as an ion-pair reagent and 15% methanol (pH 2.6), maleate of a weak acidic moiety and chlorpheniramine of a weak basic moiety in chlorpheniramine maleate were separately eluted within 10 min, and both moieties were simultaneously determined. The present approach was a useful tool for the quality control of manufactured chlorpheniramine maleate. This method was also applicable to the determination of chlorpheniramine maleate in the ophthalmic solutions.