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Synthesis of nanoparticle from biopolymers present in agricultural waste residue is significant as they are eco-friendly and serve as alternative to unrenewable petroleum resources. This research focuses on utilizing Corn cob, a lignocellulosic biomass for the simultaneous production of cellulose and hemicellulose using an energy efficient method. A sequential process of microwave irradiation and ultrasound technique is carried out to obtain cellulose and hemicellulose at a faster rate. Microwave assisted delignification showed that delignification of about 97.31% was achieved at an optimum condition of 180 W power, 12.86% Sodium chlorite and 16 min reaction time. Ultrasound assisted alkali extraction resulted in a yield of 0.445 g of cellulose /g of corn cob and 0.327 g of hemicellulose /g of corn cob at an optimum condition of 41 °C, 14% NaOH for 46 min. The extracted cellulose and hemicellulose were …