<p>In the present study, nanochitosan prepared using bottom-up (ionotropic gelation) and top-down (ball milling) approaches were compared in terms of their physical and functional properties, for the first time, to understand their characteristic difference and thereby use as potential fillers in biodegradable films. The results revealed that nanochitosan (INC) synthesized by crosslinking chitosan (C) with sodium tripolyphosphate (STTP) exhibited higher moisture content (13.22 ± 0.28)%, water absorption capacity (1365.33 ± 4.75)%, Hausner ratio (1.5 ± 0.21) and Carr’s index (30.82 ± 4.65)%, indicating INC were more hygroscopic with low flowability and high cohesiveness than nanochitosan (BNC) obtained after ball milling. However, FESEM confirmed rough-surfaced BNC and INC with an average diameter of 93.16&#xa0;nm and 66.47&#xa0;nm, respectively, while DLS showed hydrodynamic diameters of 667.46 ± 55.692&#xa0;nm for BNC and 293.4 ± 1.852&#xa0;nm for INC. Furthermore, FTIR peak shift in INC from 1649&#xa0;cm<sup>−1</sup> to 1544.44&#xa0;cm<sup>−1</sup> confirmed cross-linking of C and STTP. In addition, a decrease in enthalpy in BNC (ΔH = 272.5&#xa0;J/g) and INC (ΔH = 211&#xa0;J/g) indicated the presence of amorphous sites, while TGA showed BNC with a higher T<sub>max</sub> at 306.22&#xa0;°C and INC with higher retention of residual mass of around 35.7% at 700&#xa0;°C, indicating its stability at higher temperatures. In conclusion, the findings suggest INC is suitable for fresh produce packaging, while BNC is preferable for moisture-sensitive food. However, due to stronger ionic interactions, homogenous particle size distribution, and the ability to retain solid residue at higher temperatures, INC is a better choice in film formulations.</p> Graphical Abstract <p></p>

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Comparative Evaluation of Functional Properties and Thermal Stability of Nanochitosan Synthesized Via Ionotropic Gelation and Ball Milling

  • Payel Dasgupta,
  • Jayeeta Mitra

摘要

In the present study, nanochitosan prepared using bottom-up (ionotropic gelation) and top-down (ball milling) approaches were compared in terms of their physical and functional properties, for the first time, to understand their characteristic difference and thereby use as potential fillers in biodegradable films. The results revealed that nanochitosan (INC) synthesized by crosslinking chitosan (C) with sodium tripolyphosphate (STTP) exhibited higher moisture content (13.22 ± 0.28)%, water absorption capacity (1365.33 ± 4.75)%, Hausner ratio (1.5 ± 0.21) and Carr’s index (30.82 ± 4.65)%, indicating INC were more hygroscopic with low flowability and high cohesiveness than nanochitosan (BNC) obtained after ball milling. However, FESEM confirmed rough-surfaced BNC and INC with an average diameter of 93.16 nm and 66.47 nm, respectively, while DLS showed hydrodynamic diameters of 667.46 ± 55.692 nm for BNC and 293.4 ± 1.852 nm for INC. Furthermore, FTIR peak shift in INC from 1649 cm−1 to 1544.44 cm−1 confirmed cross-linking of C and STTP. In addition, a decrease in enthalpy in BNC (ΔH = 272.5 J/g) and INC (ΔH = 211 J/g) indicated the presence of amorphous sites, while TGA showed BNC with a higher Tmax at 306.22 °C and INC with higher retention of residual mass of around 35.7% at 700 °C, indicating its stability at higher temperatures. In conclusion, the findings suggest INC is suitable for fresh produce packaging, while BNC is preferable for moisture-sensitive food. However, due to stronger ionic interactions, homogenous particle size distribution, and the ability to retain solid residue at higher temperatures, INC is a better choice in film formulations.

Graphical Abstract