A simple bonded phase liquid chromatographic method has been described for rapid, selective and sensitive assay of chlorpheniramine maleate in human serum. The method utilized a 5 μm octadecasilane (C18) Lichrosphere RP column (250 x 4.6 mm i.d.). The mobile phase consisted of acetonitrile-methanol- 0.075 M ammonium dihydrogenphosphate (23: 9: 68%, v/v/v) at pH 2.8. Detections were carried out at 269 nm at ambient temperature. Brompheniramine was employed as an internal standard, running time per single analysis at a flow rate of 1.2 ml/min was no longer than 7 minutes. A mean absolute recovery of about 86% and a minimum detectable concentration of 0.5ng/ml of serum were obtained. The within and between-day coefficients of variation for 2.5-15ng/ml ranged from 5.96 to 8.15% and from 6.81 to 8.79%, respectively. The response of the assay over the same concentration range was linear with a mean correlation coefficient, (r), better than 0.995.