Succeeded high-temperature acid hydrolysis of granular maize starch by introducing heat-moisture pre-treatment.

Acid hydrolysis is a crucial method for modifying granular starch, but it is often conducted at low temperatures (below 55 °C) for an extended period of time to prevent crystallinity loss. The high-temperature acid hydrolysis (HTAH) behavior of heat-moisture treated (HMT) starch at 69 °C was investigated for the first time. The crystalline structure of starch was enhanced by HMT, confirmed by its rheological, thermal, and infrared Fourier transform spectroscopy results. The amorphous structure of HMT starch was preferentially hydrolyzed with high reactivity, related to a fast hydrolysis stage (4.17 × 10 min). And the crystalline flakes were separated from starch granules, accompanied by strengthened molecular interactions. HMT starch was transformed from 16.98 μm granules to 158 nm thick and 2.57 μm broad flakes with a 6.40 % increase in crystallinity after 40 min of hydrolysis. For native starch, the HTAH destroyed the crystalline structure due to gelatinization, resulting mainly gelatinous aggregates. These evidenced that the hydrolysis of granular starch was successfully performed at a relatively high temperature by introducing heat-moisture pre-treatment. This study could provide a novel perspective on the combination of increasing temperature and pre-treatment for granular starch hydrolysis intensification design, as well as a strategy for efficiently preparing small-sized crystalline starch, which has promising applications in Pickering emulsion and material filler.