This paper describes a sensitive spectrophotometric method developed for determination of Ketoconazole (KC) in tablets based on amplification reactions. Ketoconazole was oxidized with periodate, resulting in formation of KC2t and iodate ions. After masking the excess periodate with molybdate, the iodate was treated with iodide to release iodine. The liberated iodine was transformed to ICl2 species and extracted as ion-pair with rhodamine 6G into toluene for spectrophotometric measurement at 535 nm. A linear calibration graph was obtained between 0.2136 mg/mL and 1.7088 mg/mL of Ketoconazole with a molar absorptivity of 5 105 mol L 1 cm 1. The procedure was successfully applied for the determination of ketoconazole in tablet formulation. This paper describes a sensitive spectrophotometric method developed for Ketoconazole (KC) in tablets based on amplification reactions. Ketoconazole was oxidized with periodate, resulting in formation of KC2t and iodate ions. After masking the excess periodate with molybdate, the iodate was treated with iodide to release iodine. The liberated iodine was transformed to IC12 species and extracted as ion-pair with rhodamine 6G into toluene for spectrophotometric measurement at 535 nm. A linear calibration graph was obtained between 0.2136 mg / mL and 1.7088 mg / mL of Ketoconazole with a molar absorptivity of 5 105 mol L 1 cm 1. The procedure was successfully applied for the determination of ketoconazole in tablet formulation.