Storage of maize products such as tortillas may cause starch retrogradation and lead to resistant starch (RS) formation. This study was carried out to determine if storage of maize tortillas under refrigerated conditions enhanced RS content and/or modified RS structure. Improved Costeño variety maize grain was nixtamalized and processed into tortillas which were stored for five and ten days at 5°C. Total resistant starch (TRS) and retrograded resistant starch (RRS or RS3) contents were determined on raw and nixtamalized maize grain and tortillas stored for zero, five and ten days. Differential scanning calorimetry (DSC), X‐ray diffraction (XRD) and near‐infrared (NIR) spectroscopy were use to evaluate structural changes in retrograded resistant starch isolated from each sample type. Total starch content was 67 ± 1.5% for all samples, TRS ranged from 3.3% in the raw grain at 7.2% in tortillas stored for ten days, while RRS starch content ranged from 0% in the raw grain to 3.2% in tortillas stored for ten days. DSC showed endothermic transitions corresponding to amylopectin and amylose retrogradation, at 31.9 and 139.7°C in RRS from tortillas stored for five days, and at 47.9 and 146°C in RRS from tortillas stored for ten days. These values agreed with the higher total RS content recorded after prolonged storage. XRD revealed a starch crystallinity of 13.7% in tortillas stored for five days and 15.3% in those stored for ten days. NIR spectroscopy analysis showed evidence of structural changes in polymeric order that were more pronounced in RRS of tortillas stored for ten days, due to increase in crystalline region.

Raw maize, masa, and fresh and stored tortillas of white starch quality maize (Costen˜o) and common maize were analysed for chemical composition, dietary fibre, digestible (DS) and resistant (RS) starches. Changes in starch crystallinity and microstructure were also evaluated. Protein content was lower in masa and tortillas than in the original maize samples. Insoluble (IDF) and soluble (SDF) dietary fibres were higher in Costen˜o than in common maize, but stored tortillas showed the highest value in both samples. DS decreased and RS increased during tortillas storage, made with both starches. The development of RS explained the observed decrease in DS in masa (enthalpy of gelatinisation). Differential scanning calorimetry studies showed peak gelatinisation temperatures (T p ) of 75.1 and 69.4 C for Costen˜o and common maize respectively. Masa of common maize showed a second transition endotherm (T p , 108.9 C) which corresponded to amylose-lipid complexation. Tortillas with 5 and 10 days of storage showed an endothermic event at 53 and 55.7, and 54.5 and 59.9 C for Costen˜o and common maize respectively, due to starch retrogradation. These values were in accordance with the higher total RS contents recorded after prolonged storage. Microscopic structures for masa and fresh tortillas showed that the high temperature imposed on the masa and the influence of mechanical stress during tortillas making were great enough to disrupt starch granules. In general, structural changes were in agreement with changes in starch.