Syringa pubescens Turcz. has been universally employed to make flower tea for the treatment of cough in the western part of Henan Province. Many researchers have confirmed that the phenylethanoid glycosides from S. pubescens were bioactive compounds. In this study, various macroporous resins have been employed to evaluate the potential of adsorption and desorption for phenylethanoid glycosides. The HPD‐450 resins were appropriate for the purification of phenylethanoid glycosides, and the optimum purification conditions were established. The adsorption properties were well modeled using the pseudo‐second‐order kinetics. Meanwhile, the adsorption isotherm could be better represented by the Langmuir equation, suggesting that the process was an exothermic reaction. Moreover, the purified sample possessed a stronger antioxidant capacity. The inhibitory activity of the crude extract against α‐amylase and α‐glucosidase was stronger than that of purified sample. The findings obtained provided a scientific foundation for further research and high‐value exploration of this plant and a potential technique for scale‐up purification of phenylethanoid glycosides.