The catalytic activity of metal-organic frameworks (MOFs) in the degradation of environmental pollutants has garnered considerable interest recently. FTIR, FE-SEM, EDS, XRD, XPS, VSM, TEM, and N2 sorption-desorption isotherms were used to characterize Fe-based nanohybrids derived from MIL-53(Fe). In the catalytic ozonation of cefixime (CFX), the nanohybrid (CM-500) synthesized at 500°C exhibited high efficiency. The enhanced catalytic activity of CM-500 may have been caused by Lewis acid sites (LAS), iron oxides, and oxygenated functional groups of the mesoporous carbon substrate that remained after pyrolysis of the organic framework. During 15 minutes of continuous ozonation, the CM-500/O3 process was the most effective at removing CFX with a removal efficiency of 97%, significantly higher than single ozonation with a degradation efficiency of 43% under the same conditions. Modeling and optimization of process conditions were conducted using a novel and efficient class of experimental design, namely optimal design with the fewest possible runs. Calculated CFX degradation kinetic rate constants were 0.212 min-1 with CM-500, 0.043 min-1 with MIL-53 (Fe), and 0.038 min-1 for ozonation alone. Mineralization (measured COD and TOC) is significantly higher in the CM-500/O3 system compared to single ozonation. Moreover, the scavenging experiment confirmed that the reactive oxygen species in the catalytic ozonation of CFX are surface-adsorbed superoxide and hydroxyl radicals. Due to CM-500's sustained activity and magnetic properties, it is expected that it has a high catalytic capacity for treating pharmaceutical wastewater.