Using waste pomelo peel as raw material, pomelo peel-based biochar (BC) was prepared by pyrolysis at 400 °C, and the pomelo peel-based biochar was prepared by loading γ-Fe2O3 onto the surface of the pomelo peel-based biochar by unlimited oxygen chemical precipitation. The results showed that the pomelo peel biochar loaded with γ-Fe2O3 had higher specific surface area and larger pore volume. The load of γ-Fe2O3 gives γ-Fe2O3@BC excellent magnetic separation ability, and its magnetic saturation intensity is as high as 30.60 emu/g. BC and γ-Fe2O3@BC were applied to remove norfloxacin (NOR) from a water body. It was found that the adsorption of NOR by both of them followed the pseudo-second-order kinetic model. The adsorption isotherm mainly conforms to the Sips model, and the adsorption process of NOR is a spontaneous endothermic reaction. The pH and ionic strength have a great influence on the adsorption of NOR by BC and γ-Fe2O3@BC, and they play a role mainly by influencing the morphology of NOR in water. The adsorption mechanism showed that cation exchange and hydrogen bonding were the main forces for BC to adsorb NOR. Moreover, the γ-Fe2O3 particles enhanced the hydrophobicity of the pomelo peel-based biochar, making the hydrophobicity become the main force for the adsorption of NOR by the γ-Fe2O3@BC. The adsorption-desorption experiment showed that after four cycles of recycling, the adsorption capacity of γ-Fe2O3@BC for NOR was still up to 61.43% of the initial adsorption capacity, and it had a good recycling property.