Novel boronic acid-decorated metal-organic frameworks grown in situ on chitosan microspheres (CS@PD@BA-MOF) were fabricated for highly selective enrichment of cis-diol-containing nucleosides. The unique chemical properties of boric acid as ligand enable the MOF structure to form stable borate ester bond with the cis-diol-containing nucleoside, thus realizing highly selective and efficient capture of nucleoside compounds. The morphology and structure of CS@PD@BA-MOF composite was systematically characterized. The selective adsorption behavior and enrichment mechanism were investigated in details. The excellent adsorption properties of the composite also benefit from the multilayer adsorption mechanism, as well as the synergistic effect of boronate affinity, electrostatic interaction, hydrogen bond and π-π interaction, with the adsorption capacity of adenosine up to 133.15 mg g