Cereal Chem. 83(3):228-234Production of corn gluten meal (CGM), a high-protein coproduct from wet milling of corn, is increasing as production of fuel ethanol from corn increases. Unpleasant taste and odor have limited the use of CGM in human food. Adjustment of pH and extraction with water have been reported to reduce the off-flavor of CGM but the improvement is not enough for substantial addition of CGM to the human diet. More study of CGM is needed. In this study, volatile compounds released under different conditions of pH, water extraction, and temperature were identified and compared using solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). The water-extractable portion, which im-proves the taste of CGM by its absence, was dried and analyzed by SPME-GC-MS. In addition, materials extractable from CGM with methylene chloride were identified by gas chromatography-mass spectrometry (GC-MS). Further, the spontaneous generation of a CGM-like odor accompanied by a change in physical appearance of the CGM sample was described. Flavors and odors known to be associated with the identified CGM compounds were listed. Some possible origins of the volatiles, from degradation of corn constituents or as fermentation products of the corn steeping process, were noted.