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<p>Sustainable and fluoride-free alternatives for oral care products are increasingly sought. This study aimed to valorize eggshell waste as a calcium source for the synthesis of nanocrystalline hydroxyapatite (HAp) and to evaluate its suitability as a multifunctional filler in toothpaste formulations, focusing on rheological, viscoelastic, and enamel remineralization performance.&#xa0;Hydroxyapatite was synthesized from eggshell-derived calcium oxide via wet chemical precipitation and characterized using particle size analysis, FTIR, and XRD. Toothpaste formulations containing 0, 3, 5, and 7 wt% HAp were prepared. Steady shear and dynamic oscillatory rheological measurements were performed and fitted using the Herschel–Bulkley model. In vitro, remineralization was assessed on artificially demineralized bovine enamel using Vickers microhardness testing before demineralization, after lesion formation, and after treatment with HAp-based toothpaste.&#xa0;The synthesized HAp was phase-pure and nanocrystalline, with an average crystallite size of approximately 12–14 nm. All formulations exhibited non-Newtonian shear-thinning behavior with a well-defined yield stress. Increasing HAp content significantly enhanced yield stress, consistency index, storage modulus, and critical stress, indicating progressive reinforcement of the internal microstructure. The formulation containing 5 wt% HAp showed the most balanced viscoelastic properties. Artificial demineralization reduced enamel microhardness by approximately 53% compared with sound enamel. Treatment with HAp-based toothpaste significantly increased microhardness (p &lt; 0.001), restoring values to levels not statistically different from sound enamel. The calculated remineralization percentage reached 115.97%, suggesting effective mineral deposition and surface reconstruction.&#xa0;Eggshell-derived hydroxyapatite acts as both a rheological reinforcing agent and a biomimetic remineralizing material in toothpaste formulations. An optimal loading of 5 wt% provides improved mechanical integrity and controlled flow behavior while promoting substantial enamel remineralization under vitro conditions.&#xa0;This study supports the use of eggshell-derived hydroxyapatite as a sustainable biomimetic remineralizing agent for fluoride-free or fluoride-complementary toothpaste formulations, combining favorable handling properties with significant enamel remineralization potential.</p>

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Eggshell-derived hydroxyapatite as a bioactive filler for toothpaste: rheology and enamel remineralization performance

  • 期刊论文

  • 发表日期：

    2026年7月28日

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  • Bel Abbes Bachir Bouiadjra,
  • Sarah Bouameur,
  • Amine Yerou,
  • Omar Khatir,
  • Larbi Hammadi,
  • Abdelouahab Ait Kaci,
  • Mohamed Mokhtar Bouziane,
  • Mohamed. B. Bachir Bouiadjra,
  • Belaid Mechab,
  • Atef Hamada

摘要

Sustainable and fluoride-free alternatives for oral care products are increasingly sought. This study aimed to valorize eggshell waste as a calcium source for the synthesis of nanocrystalline hydroxyapatite (HAp) and to evaluate its suitability as a multifunctional filler in toothpaste formulations, focusing on rheological, viscoelastic, and enamel remineralization performance. Hydroxyapatite was synthesized from eggshell-derived calcium oxide via wet chemical precipitation and characterized using particle size analysis, FTIR, and XRD. Toothpaste formulations containing 0, 3, 5, and 7 wt% HAp were prepared. Steady shear and dynamic oscillatory rheological measurements were performed and fitted using the Herschel–Bulkley model. In vitro, remineralization was assessed on artificially demineralized bovine enamel using Vickers microhardness testing before demineralization, after lesion formation, and after treatment with HAp-based toothpaste. The synthesized HAp was phase-pure and nanocrystalline, with an average crystallite size of approximately 12–14 nm. All formulations exhibited non-Newtonian shear-thinning behavior with a well-defined yield stress. Increasing HAp content significantly enhanced yield stress, consistency index, storage modulus, and critical stress, indicating progressive reinforcement of the internal microstructure. The formulation containing 5 wt% HAp showed the most balanced viscoelastic properties. Artificial demineralization reduced enamel microhardness by approximately 53% compared with sound enamel. Treatment with HAp-based toothpaste significantly increased microhardness (p < 0.001), restoring values to levels not statistically different from sound enamel. The calculated remineralization percentage reached 115.97%, suggesting effective mineral deposition and surface reconstruction. Eggshell-derived hydroxyapatite acts as both a rheological reinforcing agent and a biomimetic remineralizing material in toothpaste formulations. An optimal loading of 5 wt% provides improved mechanical integrity and controlled flow behavior while promoting substantial enamel remineralization under vitro conditions. This study supports the use of eggshell-derived hydroxyapatite as a sustainable biomimetic remineralizing agent for fluoride-free or fluoride-complementary toothpaste formulations, combining favorable handling properties with significant enamel remineralization potential.