Novel robust metal-organic frameworks (5-FSA = N-MIL-101(Al)) was fabricated based on simple covalent binding of NH 2 -MIL-101(Al) and 5-formylsalicylic acid (5-FSA) for sensitive fluorimetric sensing of ferric ions. The structural characterization and morphology of the 5-FSA = N-MIL-101(Al) sensor were thoroughly evaluated. The novel 5-FSA = N-MIL-101(Al) sensor presented a wide linear range from 3.58 to 68.0 μM, a low detection limit (0.73 μM) with a fast response time of 15 seconds at pH 7-8. The selectivity of the developed sensor was accomplished against various competing ions and was successfully applied to the quantitative assay of ferric ions in serum and pharmaceutical tablets. The outcomes results were validated through comparison with AAS. The excellent accuracy (recovery%, 95.83-101.10) and high precision (RSD%, 1.71-2.23) indicated that the 5-FS = N-MIL-101(Al) sensor provided a high potential for fast, ultrasensitive, and selective determination of ferric ions in clinical detection with excellent reproducibility and reversibility.