Free radical therapy, based on the sulfate radical derived from peroxymonosulfate, has recently been explored as a potential cancer treatment. However, while it is promising, its successful application is restricted by several limitations including the uncontrollable generation of free radicals and the instability in aqueous medium. Herein, we prepared LCP nanoparticles by using PMS as a core, the Co-coordination polymer (Co-CP) as a coating layer, and lactobionic acid as a targeting ligand for hepatoma carcinoma cells. LCP could be activated by cobalt ions released from Co-CP, and successfully induced apoptosis and ferroptosis via the inhibition of glutathione peroxidase 4 and caused the accumulation of lipid peroxidation to enhance the efficacy of free radical therapy.