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Breeding for high-amylose corn requires a rapid method for determining starch amylose so that generating chemistry values does not pose a major limitation in the volume of materials to be screened. Two recently described methods, one an iodine-based technique involving solubilizing ground whole corn in DMSO and one based on near-infrared transmittance spectroscopy (NITS) were compared to an older technique described here as the Williams' method. The NITS method showed poor correlation to the Williams' method (r = 0.88) however, it did appear to discriminate among corn samples possessing the ae allele versus those having a normal or possibly segregating endosperm types. The DMSO-iodine method showed a much better correlation (r = 0.92) and appeared to better discriminate among samples having amylose values greater than 65% from those near 55%. Finally, this study revealed that the exotic germplasm used to develop grain sample used in the study may be an important source of genes conditioning high amylose levels since several samples having amylose values over 70% were identified.