A film of carboxymethyl‐β‐cyclodextrin‐intercalated Zn–Al layered double hydroxide (CMCD–LDH) was investigated for selective adsorption of the nucleosides adenosine (A) and guanosine (G). The effects of pH value and adsorption time on the adsorption behavior were studied. The CMCD–LDH film shows a higher selectivity for G than A under identical conditions of G and A, which results from the ability of selective recognition of the interlayer CMCD. The kinetic studies show that adsorption of A and G by the CMCD–LDH film can be described satisfactorily by the slab diffusion model. Both the values of diffusion coefficient (D) and adsorption capability (qe) of G by the CMCD–LDH film are larger than those of A, demonstrating the selective adsorption of the CMCD–LDH film for nucleosides. Due to its easy preparation and manipulation, this film is expected to be successfully applied in the field of selective adsorption and separation.