A totally green process based on reactive extrusion was used for the production of cassava starch hydrogels through reaction with two organic crosslinking agents, citric (CA) and tartaric (TA) acids. CA and TA were used at different concentrations (0, 2.5, 5.0, 10.0, 15.0, and 20.0%). Degree of substitution (DS) of hydrogels ranged from 0.023 to 0.365. Fourier transform infrared spectroscopy results showed a new band appearing at 1730 cm−1 associated with ester carbonyl groups. X-ray diffraction indicated that reactive extrusion resulted in the disappearance of diffraction peaks of native starch and samples with lower crystallinity indices ranging from 37% (native starch) to 8–11% in starch hydrogels. Morphology analysis showed that the original granular structure of starch was lost and replaced by a rougher and irregular structure. Water holding capacity values of starch hydrogels obtained by reactive extrusion were superior to those of native starch and the control sample (extruded without the crosslinking agents). Hydrogels obtained with the highest CA or TA concentration (20.0%) resulted in the higher DS and swelling capacities, resulting in samples with 870 and 810% of water retention, respectively. Reactive extrusion was effective in obtaining starch hydrogels by reaction with organic acids.
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