This research focuses on the overall extraction process of alkylresorcinols (ARs) from uncooked grains and baked products that have been processed with wheat, corn, rice, and white flour. Previously established extraction methods developed by Ross and colleagues, as well as a semiautomated method involving accelerated solvent extraction (ASE), were applied to extract ARs within freshly ground samples. For extraction of alkylresorcinols, nonpolar solvents such as ethyl acetate have been recommended for the extraction of uncooked foods, and polar solvents such as 1-propanol:water (3:1 v/v) have been recommended for the extraction of baked foods that contain rye, wheat, or other starch-rich grains. A comparison of AR extraction methods has been investigated with the application of gas chromatography and a flame ionization detector (GC-FID) to quantify the AR content. The goal of this research was to compare the rapid accelerated solvent extraction of the alkylresorcinols (ASE-AR) method to the previous manual AR extraction methods. Results for this study as well as the investigation of the overall efficiency of ASE-AR extraction with the use of a spiking study indicated that it can be comparable to current extraction methods but with less time required. Furthermore, the extraction time for ASE (approximately 40 min) is much more convenient and less tedious and time-consuming than previously established methods, which range from 5 h for processed foods to 24 h for raw grains.