A simple, precise, accurate and reproducible spectrophotometric method has been developed for simultaneous estimation of Tramadol hydrochloride (TRA) and Diclofenac Sodium (DIC) by employing first order derivative method by using methanol as solvent. The first order derivative absorption at 251.13 nm (zero cross point of Diclofenac sodium) was used for quantification of Tramadol hydrochloride and 273.75 nm (zero cross point of Tramadol) for quantification of Diclofenac sodium. The linearity was established over the concentration range of 5- 25 μg/ml in and 5-45μg/ml for Tramadol and Diclofenac sodium respectively. The correlation coefficient (R2) for Tramadol 0.9998 and for Diclofenac sodium 0.9991 .The mean % recovery was found to be in range of 99.00% and 99.68% for TRA and DIC, respectively. The proposed method fulfils the validation parameter as per ICH guidelines and was successfully applied to the estimation of TRA and DIC in bulk as well as in synthetic mixture.