Relationship of Gelatinization and Recrystallization of Cross‐Linked Rice to Glass Transition Temperature

Nonwaxy rice starch was cross‐linked with sodium trimetaphosphate and sodium tripolyphosphate to obtain different degrees of cross‐linking (9.2, 26.2, and 29.2%). The objective was to investigate the influence of cross‐linking on thermal transitions of rice starch. Starch suspensions (67% moisture) were heated at 2°C/min using differential scanning calorimetry (DSC) to follow melting transition of amylopectin. Biphasic transitions were observed at ≈60–95°C in all samples. Melting endotherms of amylopectin shifted to a higher temperature (≤5°C) with an increasing degree of cross‐linking, while there was no dramatic change in enthalpy. Recrystallization during aging for 0–15 days was significantly suppressed by cross‐linking. The delayed gelatinization and retrogradation in crosslinked starch were evident due to restricted swelling and reduced hydration in starch granules. Glass transition temperature (T_g) measured from the derivative curve of heat flow was ‐3 to ‐4°C. No significant change in T_g was observed over the storage time studied.     

Mobility and distribution of water in cassava and potato starches by 1H and 2H NMR

Mobility and distribution of water in cassava (rainy and drought crops) and potato starches were studied by solid state and NMR relaxometry as a function of H(2)O and D(2)O contents ranging from 0 to 44% (dry basis). Measurements of relative mobility derived from (2)H solid state NMR were based on relative area and line shape analysis. The narrow peak (mobile component) started to show at 5% and increased with increasing D(2)O content. This increase in mobile fraction was accompanied by a line narrowing. The mobile fractions of deuterons reached a >98% level above 15% D(2)O, which is well below the water holding capacity of starch ( approximately 27%) and the previously assigned "glassy-rubbery transition point" (24.3%; Jouppila, K.; Roos, Y. H. The physical state of amorphous corn starch and its impact on crystallization. Carbohydr. Polym. 1997, 32, 95-104). This reconfirms the liquidlike nature of water in the so-called glassy state of starch granules. The plasticization effect of water on starch chains was observed at 14-17% for cassava and potato starches as indicated by the T(1) minimum. This, however, did not seem to relate to the difference observed in swelling among the starches studied.