Abstract: In this experiment, Coix chinensis Tod. was used as raw material, the crude extract of β-sitosterol in coix seed was separated and purified by macroporous resin, and antioxidant properties of the study. By comparing the static adsorption-desorption effects of three resins, AB-8, D-101 and DA-201, Ab-8 resin as separation and purification of the best resin, the adsorption and desorption conditions of the column were optimized and scavenging ability DPPH and·OH were determined. The best conditions of β-sitosterol separation and purification were as follows:resin mass 3 g, injection concentration 0.55 mg/mL, elution speed 1 mL/min. Under these conditions, the average recovery of β-sitosterol was 85.56%±0.33%, which was close to the predicted value of 86.2707%.The purity of β-sitosterol increased from 13.8% to 76.17%. The results showed:AB-8 resin separation and purification better. Antioxidant activity indicated that β-sitosterol had good antioxidant activity.