A spectrophotometric method was developed for simultaneous quantification of pseudoephedrine hydrochloride (PSE) triprolidine hydrochloride (TRI) using second derivative method (zero-crossing technique). The second derivative amplitudes of PSE and TRI were measured at 271 and 321 nm, respectively. The calibration curves were linear in the range of 200 to 1,000 g/ml for PSE and 10 to 50 g/ml for TRI. The method was validated for specificity, accuracy, precision, limit of detection and limit of quantitation. The proposed method was applied to the assaying and dissolution of PSE and TRI in commercial tablets without any chemical separation. The results were compared with those obtained by the official USP31 method and statistical tests showed that there is no significant between the methods at 95% confidence level. The proposed method is simple, rapid and suitable for the routine quality control application. KeywordsTriprolidine, Pseudoephedrine, Derivative spectrophotometry, Dissolution testing.