Through a four-step top-down approach, native tapioca starch (NTS) was thermally acid-hydrolyzed, periodate-oxidized with subsequent removal of iodine species (i.e., IO(-), IO(-), I(-), and I), and dialdehyde tapioca starch (DTS) alcohol-precipitation. The percent yield was ∼91%. Analyses confirmed the presence of aldehydic functionalities (∼71%), effectual iodine species removal (∼98%), and enhanced water-solubility (∼96.57%). Besides, the combined treatment significantly reduced the M (∼57.81 kDa) and ameliorated homogeneity as well as thermal stability (T ∼ 667.15 °C). Structural-spectral characterization also confirmed the presence of aldehydic functionality, polymorphic transition (C- to A-type), and a higher degree of crystallinity (∼91.77%), the latter further corroborated by thermal analysis. The morphological study revealed that the combined treatment reduced size (∼393.55-nm-diameter and ∼5.22-μm-length) and changed shape into rod-like crystals. DTS showed considerably and significantly low cytotoxicity to HaCaT cells in vitro at the concentrations assayed over the test period (24 h). DTS's conformation was most stable at -289 kcal/mol and -151.7 au heat formation and minimum potential energies, respectively. Overall, these results demonstrated that the combined treatment had no deleterious effects on NTS's properties, thus yielded DTS with ideal properties for multifarious uses.
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