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Objective: To prepare iodine-131( 131 I) labeled biodegradable microspheres with chitosan and collagen for treating liver cancer., Methods: Collagen-chitosan microspheres (CCMSs) were prepared with type-Ⅰ collagen and chitosan using emulsification-chemical cross-linking method. The size of the CCMSs were determined by electron microscope. 131 I-CCMSs were achieved using Chloramine-T. The labelling rate of 131 I was recorded. The stability of 131 I-CCMSs in vitro were evaluated in PBS or human blood serum through 192 h incubation. The HepG2 model was established in nude mice 28 d after subcutaneous injection of 10 6 HepG2 cells. The model mice were sacrificed 7 d after injection of 131 I-CCMSs,blank microspheres,or PBS (five mice in each group) into the HepG2 tumor xenografts. Samples of various organs were collected to determine the distribution of 131 I-CCMSs. The curative effect of 131 I-CCMSs on liver cancer was assessed by staining with HE for histological analyses., Results: CCMSs were synthesized with a smooth and spherical shape and an average diameter of (5.1±1.2) μm. A radiolabeling rate of 86.10% was achieved. 131 I radio-loading remained stable: 92.00% in saline and 83.00% in human serum after 192 h incubation. 131 I was mainly concentrated in the subcutaneous tumor tissues. Potent curative effects of 131 I-CCMSs on subcutaneous tumor tissues were demonstrated., Conclusion: Biodegradable CCMSs were successfully prepared and radiolabeled. The 131 I-CCMSs exhibited potential curative effects on liver cancer,with high stability in vitro and in vivo., (CopyrightCopyright© by Editorial Board of Journal of Sichuan University (Medical Science Edition).)