Comparative Study of the Retrogradation of Intermediate Water Content Waxy Maize, Wheat, and Potato Starches

The retrogradation of extruded starches from three different botanical sources was studied in concentrated conditions (34 ± 1% water) at 25 °C using differential scanning calorimetry (DSC) and isothermal calorimetry, Fourier transform infrared spectroscopy (FTIR), and wide-angle X-ray scattering. Potato starch showed the highest rate of retrogradation (∼0.17 h-1) followed by waxy maize (∼0.12 h-1), while the retrogradation of wheat starch was the slowest (∼0.05 h-1). In addition to the kinetics, the extent of molecular order in the retrograded samples was studied in detail in terms of “short-range” (helical) and “long-range” (crystalline) distance scales. The amylopectin crystallinity indices were essentially the same (∼47−51% amylopectin basis) for the three starches. However, significant differences were found in the enthalpy of melting measured by DSC after “full” retrogradation (potato, 11.6 ± 0.7; waxy maize, 9.0 ± 0.5; and wheat, 6.1 ± 0.3 J/g of amylopectin). The degree of short-range molecular order in the retrograded state determined by FTIR was waxy maize > potato > wheat. The effect of amylopectin average chain length and the polymorphism of the crystalline phase were taken into account to explain the differences in the retrogradation enthalpies. Keywords: Starch retrogradation; amylopectin; isothermal calorimetry; molecular order; staling