The lignan oxomatairesinol was synthesized from the biomass-derived lignan hydroxymatairesinol via selective aerobic oxidation over a heterogeneous gold catalyst. The catalyst was prepared by direct ion-exchange and characterized by XRD, TEM and ICP-OES methods. The reaction was carried out at 70 °C and atmospheric pressure in a semi-batch reactor. To reveal the origin of catalyst deactivation, spent catalysts were studied by TEM, XRD, nitrogen physisorption, ICP-OES, TPO, and DSCTGA techniques. Several regeneration procedures were applied-extraction by several solvents and calcinations in the oxidizing atmosphere. The former one was found to be the most effective way for the catalyst regeneration.