A superfast, room-temperature, one-step carrier-solvent-assisted interfacial reaction process was developed to prepare Ag/AgFeO2 composite nanocrystals (NCs) of less than 10 nm in size within a 1 min reaction time. These composite NCs were with a direct energy band gap of 2.0 eV and were paramagnetic, making them suitable for optical activation and magnetic manipulation. These composite NCs, applied as a photocatalyst for the treatment of HeLa cells, achieved a significant reduction of 74% in cell viability within 30 min. These Ag/AgFeO2 composite NCs proved to be a promising magnetically guidable photocatalyst for cancer cell treatment.