A method for preparing corn fiber oil involving separating corn fiber from corn kernels (e.g., by a wet milling process), drying the corn fiber, grinding the dried corn fiber to produce ground corn fiber having a particle size of less than about 100 microns, combining the ground corn fiber with an aqueous solution having a specific gravity effective to float aleurone cells, removing the floating aleurone fraction, drying the aleurone fraction to form a dried aleurone fraction, grinding the dried aleurone fraction to form a ground aleurone fraction, extracting corn fiber oil from the ground aleurone fraction by a way selected from the group consisting of an organic solvent and supercritical fluid extraction, and separating the extracted corn fiber oil from the extraction medium. Also shown is a method of recovering corn aleurone cells from corn fiber involving separating corn fiber from corn kernels by a wet milling process, drying the corn fiber, grinding the dried corn fiber to produce ground corn fiber having a particle size of less than about 100 microns, combining the ground corn fiber with an aqueous solution having a specific gravity effective to float aleurone cells, and removing the floating aleurone fraction.