A novel method for regeneration of fatty acid adsorbed gamma-alumina using supercritical methanol was developed. This method is based on a difference in the affinity of a fatty acid and the corresponding fatty acid methyl ester (FAME) for gamma-alumina. Palmitic acid was selected as a model fatty acid. Batch-type reactors were used to investigate the effect of the operating parameters (temperature, methanol to gamma-alumina weight ratio, and reaction time) on supercritical methanol regeneration. Almost all of the adsorbed palmitic acid was desorbed at temperatures above 300 degrees C, or when the weight ratio of methanol to gamma-alumina was higher than 75:1, and/or if the reaction time was longer than 15 min. The crystal structure and BET surface area of y-alumina were unchanged after supercritical methanol regeneration. The developed technique requires relatively lower operating temperature, is ecofriendly, and generates fuel, although the process is more complex than the thermal regeneration method.