Influence of botanical source and gelatinization procedure (autoclaving or boiling) on resistant starch (RS) formation was investigated in starches from wheat, corn, rice, and potato. RS yields did not vary within the same sample but differed among samples with different starch botanical sources. Differences also existed in RS contents in native and retrograded starches. Slight or minor variations in RS values were found after both gelatinization procedures, although no clear pattern was found in the behavior of samples based on gelatinization procedure. The degree of polymerization (DP) of retrograded samples was assigned using high-performance anion exchange chromatography with pulsed amperometric detector (average DP 50-60), with no differences between autoclaved and boiled samples.