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Objective:In the medium of ethanol(non-polar), STMP and ADH as crosslinkers to HA, to prepare drug delivery microspheres by getting stable cross-linked products without a gel phase, and to study biocompatibility and biodegradability of cross-linked products. Methods:ISO10993.1-Safety Evaluation of Biomedical materials as a reference, to make hemolysis test, percutaneous stimulation test, acute toxicity test,and analyze in vitro degradation test,and degradation products. Results:HA-STMP cross-linked product had no hemolysis, no irritation, no acute systemic toxicity, but HA-ADH had a mild skin irritation and adverse acute systemic toxicity. HA-STMP cross-linked product had lower sensitivity on HAse and the curve is flatting. With the increase of degradation time HA-STMP results were changed by the structure analysis,degradation products of these cells were no toxicity. Conclusion:HA-STMP cross-linked products with better biocompatibility and better resistance to hydrolysis could delay the degradation time, which is suitable for the preparation of biodegradable drug carriers.