The retrogradation of extruded starches from three different botanical sources was studied in concentrated conditions (34 +/- 1% water) at 25 degrees 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 (approximately 0.17 h(-1)) followed by waxy maize (approximately 0.12 h(-1)), while the retrogradation of wheat starch was the slowest (approximately 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 (approximately 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.
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