An accurate, specific and precise assay using Reverse-phase high-performance liquid chromatography following isocratic solvent delivery system was performed for simultaneous determination of Acetaminophen and Methocarbamol in bilayered tablet dosage form formulated by us. A Develosil ODS-MG-5 column having 100×4.6mm internal dimensions was used as stationary phase and Milli Q water, Methanol & Glacial acetic acid in the ratio of 600:400:15 as mobile phase. The flow rate was 1.0ml/min & effluent monitored at 273nm.The retention times of Acetaminophen & Methocarbamol were found to be 1.846 and 4.713 min. respectively