Various starches of different AM contents and origins such as wx maize, normal maize, high AM maize, potato, and mungbean starches were hydrolyzed using a H 2 SO 4 solution (3.16 M) at 408C for 7 days, and the starch particles were isolated from the hydrolysates by centrifugation. The hydrolysis rates varied from 61.4 to 90.9% depending on the starch type. Unexpectedly, A-type starches were more resistant to the acid hydrolysis than B-type starches. XRD results revealed that the starch particles with B-crystalline type exhibited a decrease in peak intensity. In addition, in a DSC analysis, the crystals remaining in the B-type starch particles were readily disrupted in the water dispersion so that no melting endotherm appeared. Electron microscopy confirmed that the starch particles had round or oval shapes with diameters ranging from 40 to 70 nm, which possibly represented the starch blocklets in granules. The acid degraded mainly AM and long AP chains, resulting in increasing the proportion of short chains.

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Small starch particles were prepared by hydrolyzing waxy rice starch using α‐amylase and then ultrasonicating in ethanol. Differential scanning calorimetry (DSC) revealed that a mild hydrolysis for 3 hr increased the melting enthalpy of the starch, which might indicate that the hydrolysis was selective in the amorphous regions. Later, at 6–24 hr, the hydrolysis rate was reduced, with gradual decreases in DSC melting enthalpy, indicating that the crystalline regions were eroded simultaneously. X‐ray diffraction patterns revealed the same trend as the DSC results. Average diameter of starch granules or particles was decreased dramatically in both volume‐ and number‐based measurements (5.94→1.64 μm, and 0.45→0.18 μm, respectively) during the early stage of rapid hydrolysis (up to 3 hr). Native waxy rice starch exhibited a particle size distribution with a major peak at 5.6 μm. After hydrolysis for 3 hr, the volume distribution of starch granules changed to two major size peaks at 0.5 and 3.6 μm. The starch fragment of 0.5 μm was assumed to consist of crystalline blocklets. With excessive hydrolysis (24 hr) or ultrasonication, however, starch particle diameter was increased, indicating that the particles might be swollen or aggregated into clusters.