The increasing interest in the development of renewable energy sources such as biogas or bioethanol has led to study different lignocellulosic biomass as feedstock. In this work, corn biomass (stalk and leaf) was used to obtain total reducing sugar (TRS) and evaluate its suitability as feedstock for biofuels production. Biomass characterization was carried out by high performance liquid chromatography (HPLC) technique in order to determine main components (cellulose, hemicellulose, and lignin). For TRS quantification, different biomass particle size (0.5 mm, 1 mm, 2 mm, and in natura) were considered and the effect of alkaline pretreatment was studied in corn stalk, corn leaf, and corn stalk/leaf biomasses. It was found that corn cultivation wastes biomass exhibited high cellulose content of 28.38 g/L and 19.02 g/L for stalk and leaf, respectively. In addition, the highest concentration of TRS (28.89 g/L) was achieved using pretreated stalk/leaf biomass with 0.5 mm particle size indicating that alkaline pretreatment improves the TRS concentration. These results suggested that corn crop residues are an attractive feedstock for producing biofuels.