ObJective: To investigate the purification processes of Scutellaria from Sanhuang spray with macroporous adsorption resin. Method: The content of baicalin was measured with HPLC. The adsorption rate and desorption rate were measured to evaluate the optimal macroporous adsorption resin and the optimal purification conditions. Result: The optimal macroporous adsorption resin was SP-825. The optimal purification condition was as follows: the sample concentration was 0.2 g ·mL-1; the diameter height ratio was 1 ∶7; the sample volume was 2 BV; the eluant was 70% ethanol; the elution flow rate was 3 BV ·h-1; the ethanol consumption was 6 BV. Conclusion: Purification process of the extract of Scutellaria and Gardenia with SP-825 macroporous adsorption resin was stable and feasible.