The adsorption of biogenic hydroxymethylfurfural and fructose from aqueous phase reaction mixtures on polymer-based spherical activated carbons was studied. The adsorbents show a high capacity in combination with an outstanding selectivity due to their hydrophobic surface. Equilibrium isotherms and breakthrough curves of single and multicomponent solutions as well as the desorption behavior were measured and modelled accordingly. Overall, the results obtained enable further process development for adsorptive liquid phase separation in future biorefinery processes.