Magnetic iron oxide nanoparticles (MIONPs) were synthesized using tannic acid and characterized by Raman, FTIR, UV, and DRX spectroscopy. In a heterogeneous Fenton-like reaction, the catalytic peroxidase-like activity of MIONPs in the degradation of Acid Red 1 (AR 1) dye was investigated. TEM/STEM was used to determine the quasi-spherical morphology and particle size (3.2 nm) of the synthesized MIONPs. The XRD powder patterns were indexed according to the reverse spinel structure of magnetite, and SEM-EDS analysis confirmed their chemical composition. At pH = 3.5, the decomposition of H2O2 in hydroxyl radicals by MIONPs results in high AR 1 degradation (99%). This behavior was attributed to the size and surface properties of the MIONPs. Finally, the Surface Enhanced Raman Spectroscopy (SERS) technique detected intermediary compounds in the degradation process.