To optimize the technical parameters for separating phlorizin from Lithocarpus polystachyus Rehd., phlorizin extracting solution of Lithocarpus polystachyus Rehd. was used as material, static adsorption and desorption capacities of eight types of macroporous resin including D101, X-5, ADS-7, S-8, AB-8, NKA-9, HPD-100 and HPD-400 to phlorizin were analyzed. The results showed that S-8 had greater adsorption and desorption capacities to phlorizin, which was 14.70 mg/g and 8.395 mg/g, respectively. When considering the maximum phlorizin yield, the optimal concentration, flow rate and volume of phlorizin solution was determined to be 0.9 mg/mL, 3 BV/h and 7 BV, respectively; the optimal concentration, flow rate and volume of the eluent was determined to be 60%, 4 BV/h and 3 BV, respectively, and the yield was 89.89%, which was 1.76 times more than the original solution, while the purity rate was 10.50%. Whereas when considering the maximum phlorizin purity, the optimal concentration, flow rate and volume of phlorizin solution was determined to be 0.9 mg/mL, 3 BV/h, 7 BV, respectively; the optimal concentration, flow rate, and volume of the eluent was determined to be 70%, 3 BV/h and 3.5 BV, respectively, and the purity rate was 13.51%, which was 2.56 times more than the original solution, while the yield was 83.26%.