Lignocellulosic biomass is a widespread and renewable alternative to fossil resources from which valuable products such as biofuels and chemicals can be obtained. The usual biotechnological way of lignocellulose processing involves pre-treatment of biomass and enzymatic hydrolysis of complex carbohydrates (cellulose and hemicellulose) to simple sugars. The aim of this study was to examine the effect of microwave pretreatment on lignocellulosic degradation of corn cob. Biomass will be treated in a microwave oven (Bosch Serie 2, Germany) using hydrogen peroxide, under different conditions (pH and treatment time). After treatment, the solid fraction was subjected to enzymatic hydrolysis using the commercial enzyme CellicCTec2 (Novozymes, Denmark). The effect of the treatment was determined by determining the surface area of cellulose and lignin (based on the equation of Langmuir adsorption isotherm for adsorption of Congo red and Azure B, respectively), and the crystallinity index (iodine adsorption method). Enzymatic hydrolysis of biomass was monitored using spectrophotometric methods to determine the concentration of reducing sugars (DNS method), total hexose sugars (Antron method) and total pentose sugars (Orcinol method). The results of the treated samples were compared with the untreated ones in order to determine the most efficient treatment conditions for the degradation of lignocellulosic biomass.