Kinetics of structural changes in starch retrogradation observed by simultaneous SANS/FTIR-ATR measurements

Hirata, Yoshinobu*; Kaneko, Fumitoshi*; Radulescu, A.*; Nishizu, Takahisa*; Katsuno, Nakako*; Imaizumi, Teppei*; Motokawa, Ryuhei   ; Kumada, Takayuki   ; Nakagawa, Hiroshi   

A simultaneous measurement system of SANS/FTIR-ATR was applied to record multiple structural changes in potato starch during retrogradation. In the SANS patterns, the shoulder-like peak becomes more pronounced with time. The peak intensity, Imax, which represents the amount of orderly arranged double helical structures, increased over time, showing that starch reassembled orderly on the nanoscale upon retrogradation. In the FTIR-ATR spectra, the increase of the ratio of absorptions at 1042 cm and 1016 cm, indicating the amount of short-range ordered structure in starch increased during retrogradation. The time to obtain half of the equilibrium value for was larger than that for Imax. Changes in the short-range ordered structure of starch were observed to converge prior to changes in the nanostructure. These results indicate that the double-helix structures are initially formed by amylopectin side chains, and then these double-helical structures are arranged orderly.