Subzero Glass Transition of Waxy Maize Starch Studied by Differential Scanning Calorimetry

A mixture of waxy maize starch and water (1:2, w/w) was heated in a differential scanning calorimeter (DSC) pan to different temperatures to obtain different degrees of gelatinization. Each pan was then quenched to ‐30°C and rescanned, and the subzero glass transition temperature (T_g′) of the content was determined. A three‐phase model of a starch granule—a mobile amorphous phase, a rigid amorphous phase, and a crystalline phase—was used to interpret results and explain the glass transitions in starch. Waxy maize starch had an onset gelatinization temperature (T_o) of 61.5°C, peak temperature (T_p) of 70.3°C, and completion temperature (T_c) of 81.7°C. The T_g′ was clearly noted after the starch and water mixture was heated to T_p and T_c, but was small and barely observable when the mixture was heated up to T_o and immediately cooled to ‐30°C. When the starch and water mixture was heated to 55°C, which was 6°C below the T_o, and held for 2 h, a T_g′ was observed. Moreover, T_g′ began to appear and was observable if the starch and water mixture was heated to 10°C below gelatinization onset temperature (51°C) and annealed for 2 h without any gelatinization. Further holding at ‐7°C showed a clear subzero glass transition of annealed native starch granules.