Retrogradation is a critical step in the physical production of resistant starch. This study aimed to examine the effects of isothermal and temperature-cycled retrogradation on the structural, physicochemical properties, and digestibility of resistant starch type-III (RS3) under various thermal conditions. To create RS3, normal maize starch (NM) and Hylon VII (HAM) were treated by autoclave-microwave and then retrograded at isothermal (4 °C) or various temperature conditions (4/10 °C, 4/20 °C, 4/30 °C, 4/40 °C, and 4/50 °C). We found that temperature-cycled retrogradation possessed greater potential than isothermal retrogradation for producing short-range ordering and crystalline structures of RS3. Also, retrograded starch prepared via temperature cycling exhibited higher double helix content, lower amorphous content, reduced swelling power, and less amylose leaching in water. Furthermore, the starch digestibility was affected by structural alterations, which were more significant in HAM-retrograded starch. While, HAM-4-40 (39.27 %) displayed the highest level of resistant starch (RS).
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