Two simple and sensitive spectrophotometric methods were developed for the determination of paracetamol (I) and ascorbic acid (II) in pharmaceutical binary mixture. The first method depends on the use of the first-derivative spectrophotometric technique for the simultaneous determination of components of the mixture. The second method depends on the reaction of the studied drugs with 5-diazo-1, 2, 4-triazol-3-carboxylic acid (DTCA) reagent to give colored products measured at 480 nm and 380 nm for (I) and (II), respectively. All variables affecting reaction conditions were optimized. The proposed methods were successfully applied for the analysis of the studied drugs in their pure and commercial dosage forms and are in good agreement with those obtained from the reported methods. No significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. Molar ratios of the drugs with the colorimetric reagent (DTCA) were determined and the reaction mechanisms were suggested.