Currently, electrochemical sensors are in the process of being developed and widely used in various fields, and new materials are being explored to enhance the precision and selectivity of the sensors. The Fe/graphene nanoparticles were synthesized utilizing a green approach, wherein leaf extract was employed as the reducing agent. The resulting materials underwent comprehensive characterization utilizing a range of contemporary techniques, including scanning electron microscopy (SEM), X‐ray diffraction (XRD), Fourier‐transform infrared spectroscopy (FTIR), and Raman spectroscopy. The findings of the study revealed that the nanocomposites of Fe/graphene/porphyrin comprised zero‐valent iron nanoparticles, exhibiting an average particle size ranging from 15 to 60 nm. These nanoparticles were seen to be evenly dispersed across the graphene sheets. The presence of nanostructure porphyrin nanofibers, measuring 20 nm in diameter, was also shown to exhibit strong integration with the surface of the Fe/graphene nanomaterials. The electrochemical properties of the Fe/graphene/porphyrin nanocomposite were also investigated, demonstrating that the prepared material could be effectively employed as a sensing electrode in the electrochemical sensor for detecting Chloramphenicol (CAP) through CV, EIS, and DPV techniques using a three‐electrode electrochemical system. Under optimal conditions, Fe/graphene/porphyrin exhibited a high current response when detecting CAPs.