A two-step process is evaluated to separate the hexose component in wet milling corn fibers from the pentose component for production of value-added products. Corn fibers were first pretreated with hot water at 121 degrees C for 1 h followed by glucoamylase hydrolysis to remove starch. The remaining solid was then treated with hot water at 140-170 degrees C followed by an enzymatic hydrolysis to further separate the hexose and pentose components. After the second pretreatment, the enzymatic digestibility of cellulose was much better than that of arabinoxylan. As a result, up to 90% arabinoxylan in corn fibers was retained in a solid form after the enzyme hydrolysis, while most of the hexose components were removed.