Easy, precise, and accurate three spectrophotometric procedures for successive resolution of febuxostat and diclofenac potassium in their multi-ingredient formula without prior separation were established and validated. Second derivative (2 D), dual-wavelength (DW), and ratio subtraction (RS) are the names of these procedures. They showed good linearity in the ranges of 2.0-20.0 µg/mL for febuxostat and 5.0–50.0 µg/mL for diclofenac potassium with strong determination coefficients (r2 ). For 2 D (r2 = 0.9995 - 0.9998), DW (r 2 = 0.9997 -0.9998) and RS (r2 = 0.9995 - 0.9999) for febuxostat and diclofenac potassium; respectively. By using the proposed procedures, the limits of detection and the limits of quantitation for febuxostat and diclofenac potassium were 0.135–0.580 µg/mL and 0.408–1.756 µg/mL, respectively. They were also successfully used to test two drugs in their multi-ingredient formula, with the findings being checked, statistically analyzed, and found to be consistent with those obtained by a previously published method.