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In this study, hard corn grains were nixtamalized (alkali-heat treatment) by a high-energy ball mill to investigate the effects on its physicochemical, textural, and microstructural properties. Ball milling modifies the structure and properties of cornstarch. The gelatinization peak of starch was evidenced and thermal and pasting properties were significantly affected. With regard to rheological properties, the viscosity peak increased from 2454 cP in traditional nixtamalized flour to 4294 cP in high-energy milling treatments with 1.4% of Ca(OH) 2 and 20% moisture content, C1.4, while enthalpy ranged from 3.5 to 0.34 J/g, respectively. High-energy milling influenced the Fourier-Transform InfraRed Spectroscopic (FT-IR) patterns. All of the samples of the corn-grain starches presented the typical A-type X-ray diffraction pattern. The crystallinity of starch from CG showed a lower intensity in peaks 2θ ~ 15 and 23° compared with starch from WG and YG. The textural properties of the masas were influenced, adhesiveness was reduced, but cohesiveness was increased by the addition of Ca(OH) 2 . In the structural characterization by E-SEM, the control presented a greater amount of agglomerated starch granules, followed by the high-energy milling treatments. The results suggest that high-energy alkaline milling could be a potential physical and chemical method to modify corn-starch properties and obtain nixtamalized products., Competing Interests: Declaration of competing interest The authors declare that they have no conflict of interest., (Copyright © 2020 Elsevier B.V. All rights reserved.)