This research aimed to evaluate the gelation process of ferulated pectin (FP) and ferulated arabinoxylan (AXF) in a new mixed hydrogel and determine its microstructural characteristics. FP from sugar beet (Beta vulgaris) and arabinoxylan from maize (Zea mays) bran were gelled via oxidative coupling using laccase as a crosslinking agent. The dynamic oscillatory rheology of the mixed hydrogel revealed a maximum storage modulus of 768 Pa after 60 min. The scanning electron microscopy images showed that mixed hydrogels possess a microstructure of imperfect honeycomb. The ferulic acid content of the mixed hydrogel was 3.73 mg/g, and ferulic acid dimer 8-5' was the most abundant. The presence of a trimer was also detected. This study reports the distribution and concentration of ferulic acid dimers, and the rheological and microstructural properties of a mixed hydrogel based on FP and AXF, which has promising features as a new covalent biopolymeric material.