Aiming at the problems of herb residue waste, abundant impurities in crude extracts and poor selectivity of traditional purification methods in the traditional Chinese medicine extraction industry, this study established a two-step purification process combining preliminary separation by macroporous resin and deep refining with UiO-66-NH₂ for total flavonoids from Angelica dahurica. Total flavonoids were extracted via ultrasound-assisted extraction with 70% ethanol, and the content was quantified by rutin colorimetry. Five types of macroporous resins were screened to prepare crude flavonoid sample Group A. UiO-66-NH₂ was synthesized by solvothermal method and characterized by FT-IR and SEM to investigate its adsorption selectivity, adsorption kinetics and cyclic stability. High-purity flavonoid sample Group B was obtained after secondary refining. The results showed that the two-step purification effectively improved the purity of the product. The refined sample exhibited stronger antioxidant activity and tyrosinase inhibitory activity with stable moisture absorption and retention performance, which can be applied as cosmetic raw materials. The two-step purification process developed in this study provides a reference for the pharmaceutical development of high-purity Angelica dahurica flavonoids, and offers ideas for further research on resource utilization of herb residues.