An eco-friendly procedure was developed for dual detection of drug norfloxacin (NOR) and iron(III) ions in biological and pharmaceutical samples via the coupling of cloud-point extraction procedure with molecular spectrophotometry. The drug norfloxacin reacts with Fe(III) ions in dilute acidic medium to form a colored hydrophobic (Fe(III)-NOR) complex which initially extracted into micelles of Triton x-114 as a mediated extractant followed the determination of both NOR and Fe(III) ions individually, by using spectrophotometry at same wavelength maximum of 432 nm. To achieve this goal, all experimental variables for both target analytes were previously optimized. The results have shown that the preconcentration factors of 83 and 71 for NOR and Fe(II) leading to achieve a limit of detection of 0.692 μg mL -1 3.42 ng mL -1 with linear range of 2.5-125 μgmL -1 (r= 0.9998) and 5-150 ng mL -1 (r=0.9997) respectively. The mean recovery percentage of 98.95±1.09% and 98.77±2.29%; the precision (RSD%) ranged between 0.04-0.66% and 0.59-0.97% were obtained for NOR and Fe(III) respectively. The proposed method was used for the determination of NOR in the serum samples of different subjects orally administration for two hours with Norfloxacin tablets BP 400 mg, in addition to drug formulations like Norflox Eye/Ear drops, While iron was determined in four selected drug formulations and in both cases, the experimental values are agreed with the quoted values that stated by the manufacturer company,