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Corncobs of four different corn varieties were physically segregated into two different anatomical portions, namely the corncob outer (CO) and corncob pith (CP). The biomass composition analysis of both the CO and CP was performed by four different methods. The CP showed a higher carbohydrate and lower lignin content (83.32% and 13.58%, respectively) compared with the CO (79.93% and 17.12%, respectively) in all of the methods. The syringyl/guaiacyl (S/G) ratio was observed to be higher in the CP (1.34) than in the CO (1.28). The comprehensive physical characterization of both samples substantiated the lower crystallinity and lower thermal stability that was observed in the CP compared to the CO. These properties make the CP more susceptible to glycanases, as evident from the enzymatic saccharification of CP carried out with a commercial cellulase and xylanase in this work. The yields obtained were 70.57% and 88.70% of the respective theoretical yields and were found to be equal to that of pure cellulose and xylan substrates. These results support the feasibility of the tailored valorization of corncob anatomical portions, such as enzymatic production of xylooligosaccharides from CP without pretreatment combined with the bioethanol production from pretreated CO to achieve an economical biorefinery output from corncob feedstock.