Technical Abstract: Production of corn gluten meal (CGM), a high-protein coproduct from wet milling of corn, is increasing as production of fuel ethanol from corn increases. The unpleasant taste and odor of CGM has prevented widespread acceptance of this high protein commodity in human food. We previously identified a number of odorant compounds in headspace volatiles of corn gluten meal and wet cake (dryer feed). In this study, CGM volatiles at sequential stages of treatments known to improve CGM flavor were compared by solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). Headspace volatiles of the water soluble solids extracted from CGM by these treatments were identified by SPME-GC-MS. Direct injection GC-MS identified 22 components in methylene chloride extracts of CGM odors which had been further partitioned into hexane and water soluble fractions. Three classes of carotinoid degradation products associated with flavors were identified in wet cake and corn gluten meal. Knowledge of the changes in odor volatiles during treatments of CGM and knowledge of extractable odor and flavor compounds in CGM may aid in eventual identification of pathways creating off flavor and odor. This information can guide development of industrial processing methods for improvement of taste and increased utilization.