The acceptability of whole grain flours during storage varies widely, as does the estimated shelf life of such flours, in part because acceptability is typically determined using subjective human sensory testing. Research is needed to establish more objective measures of acceptability. This study correlated the quantitative results of a descriptive odor sensory panel with volatile compounds determined by solid-phase microextraction-gas chromatograph-mass spectrometry (SPME-GC-MS). Whole wheat flour and quinoa flour were held at 40°C for up to 24 weeks to accelerate changes occurring during storage. Samples were collected every 4 weeks and placed in frozen storage. Thawed samples were then evaluated using SPME-GC-MS and descriptive sensory odor analysis. Significant correlations were found between 1-hexanol, 2-pentylfuran, phenol, hexanoic acid, and hexanal volatiles of whole wheat flour and the odor descriptor cardboard/stale. This indicates that SPME-GC-MS can be used as a less expensive, less time-consuming, more precise method to determine the acceptability of whole wheat flour during storage. Significant correlations were not present in the quinoa flour data, suggesting that SPME-GC-MS may not be preferable to human sensory odor analysis in determining acceptability of stored quinoa flour.