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Surface-initiated atom transfer radical polymerization was successfully used to prepare 4-vinylphenylboronic acid functionalized poly(glycidylmethacrylate-co-ethylenedimethacrylate) beads for the selective enrichment of glycoprotein from complex biological samples in this study. The modified bead surfaces were characterized using Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The sorption behaviors, including adsorption isotherms, incubation time, and pH effect, were investigated. The results demonstrated that the boronated beads have a high affinity for glycoprotein, which is due to the well-defined boronic acid brushes on the beads surfaces. Furthermore, the polyvinylphenylboronic acid grafted poly(glycidylmethacrylate-co-ethylenedimethacrylate) beads were used to efficiently enrich and purify glycoprotein from real egg white samples and α-fetoprotein from human serum samples. The mass spectrometry results demonstrated that the polyvinylphenylboronic acid grafted poly(glycidylmethacrylate-co-ethylenedimethacrylate) beads are a suitable material for the enrichment of glycosylated protein from complex biological samples. [ABSTRACT FROM AUTHOR]