Purpose: To study the preparation technique of a sustained-released microsphere (LSD/NTCD-ACM) and evaluate its characteristic and effects for transarterial hepatic chemoembolization (TACE) in an animal model of liver cancer (VX2).Mmethods: We prepared LSD/NTCD-ACM through the emulsification-gelation method with liquid paraffin as oil phase, the hybrid of chitosan and sodium alginate as water phase, Span-80 as emulsifier, and glutaraldehyde as cross linking agent. Studied its in vitro release in pH 7.4 PBS by dynamic dialysis method.Then 24 male New Zealand white rabbits were randomly divided into four groups with 6 rabbits assigned to each group.VX2 carcinoma tissues were implanted into the left hepatic lobe using a 16g biopsy gun. The tumors were allowed to grow for weeks, and studies were performed until the volume of the tumors detected by ultrasonograph reached 2-3 cm3. Under anesthesia, transcatheter hepatic arterial embolization was performed and LSD/NTCD-ACM(60-120μm), LSD/NTCD-ACM(120-200μm) or NCTD solution was injected into the hepatic arteries of animals in the three treatment groups and the left one is control group(with no treatment).Before and at 3,7,14 days after injection, the volume of the tumor was measured by ultrasonograph, the serum of all rabbits was collected, and the level of aspartate aminotransferase (AST) was checked. During the last course of their disease, the rabbits were given analgesics to relieve suffering. The survival period of the three groups of rabbits after treatment was recorded, and degree of liver cell necrosis was also assessed on the histopathological specimens. Results: The drug entrapment efficiency (EE％) of LSD/NTCD-ACM(60-120μm) was 74.62％ and drug-loading (DL％) amount was 7.46％ while 86.93％ for EE and 9.23 ％for DL of LSD/NTCD-ACM (120-200μm) .Both the two particles could release as long as 20 days in pH 7.4 PBS. The tumor growth rate in the LSD/NCTD-ACM (60-120/μm) group (7.76±0.41, tumor volume from2.48±0.25 to19.24±1.33 cm3) and in the LSD/NCTD-ACM (120-200/μm) group (9.56±0.37, tumor volume from2.63±0.55 to 21.13±1.34 cm3) was significantly decreased compared to that in the control group(15.50±1.17, tumor volume from2.38±0.56 to36.93±1.41 cm3)(P < 0.05) and in the NCTD group (13.37±1.63, tumor volume from2.57±0.21 to 34.41±1.68 cm3)(P<0.05).The survival period and life prolonging rate in LSD/NCTD-ACM (60-120/μm)group (39.49±0.51 days, 43.81±4.34％) (P<0.05) and LSD/NCTD-ACM (120-200/μm) group(43.37±0.45 days, 57.94±5.76％)(P<0.05) was significantly longer than that in both control group(28.46±0.61 days，0％) (P<0.05) and NCTD group (26.67±0.58 days, -0.03±4.55％) (P<0.05). There was an increase (P< 0.05) in the serum AST level in the three treated group at the first day after injection when compared to the control group.And the serum AST level in the two embolization groups were higher than that in the NCTD group(P<0.05), however, no significant difference was observed between the two groups at the first day after injection (P > 0.05). Liquefaction necrosis and coagulation necrosis were both observered in the two embolization groups. Conclusion: The results of this investigation show that LSD/NCTD-ACM are potential candidates for embolization of liver cancer. And considered to its safety, the dosage of LSD/NCTD-ACM(60-120/μm) used should be further evaluated.