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Synthesis and characterization of calcium-releasing elastomeric resin-based endodontic sealers

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Abstract

Objectives

To evaluate the incorporation of halloysite nanotubes (HNTs) loaded with one of two calcium sources (i.e., calcium hydroxide/CaOH2 or beta-tricalcium phosphate/β-TCP) on the physicochemical and biological properties of an experimental resin-based dual-cured endodontic sealer.

Materials and methods

HNTs were encapsulated with CaOH2 or β-TCP at 10 wt.%. HNTs containing CaOH2 or β-TCP were added into the experimental sealers at 50 wt.%. The control sealers were the calcium-free HNT-modified resin-based experimental sealer and AH Plus™, a commercially available endodontic sealer. Degree of conversion, setting time, flow, film thickness, radiopacity, dimensional stability, and calcium ions release were determined. Antibiofilm properties and cytocompatibility of the formulated sealers and commercial control were also evaluated. One and two-way ANOVA analysis followed by Tukey’s post hoc test was conducted to evaluate the effect of the independent variable on the evaluated properties.

Results

FTIR confirmed the encapsulation of calcium sources into HNTs. Regarding flow and film thickness, the values obtained from these sealers were in accordance with the specifications provided by ISO 6876. For radiopacity, AH Plus™ achieved the highest radiopacity (p<0.05). Among the experimental formulations, all experimental HNT-containing compositions exhibited values below 3 mm Al. The experimental sealers showed greater dimensional changes when compared to the commercial (AH Plus™) control. The release of calcium ions was observed for the HNT_CaOH2 and HNT_β-TCP sealers without statistical differences. Experimental sealers containing HNT_CaOH2 and HNT_β-TCP significantly reduced the CFU/mL count and showed cell compatibility.

Conclusions

The findings of this study demonstrate that the incorporation of HNT_CaOH2 or HNT_β-TCP into resin-based experimental sealers promoted antimicrobial effects and gradual calcium release without impairing cytocompatibility or physicochemical properties of the sealers. Still, an adjustment to reach the minimal radiopacity established by ISO 6876 is needed.

Clinical relevance

The experimental resin-based sealers seemed to be an alternative for endodontics. The incorporation of calcium sources exerts promising antimicrobial effects while displaying low cell toxicity.

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Authors and Affiliations

  1. Department of Cariology, Restorative Sciences, and Endodontics, University of Michigan School of Dentistry, Ann Arbor, MI, 48109, USA

    Juliana S. Ribeiro & Marco C. Bottino

  2. Department of Restorative Dentistry, School of Dentistry, Federal University of Pelotas, Pelotas, RS, Brazil

    Juliana S. Ribeiro, Samantha R. Xavier, Fernanda G. Pappen, Evandro Piva & Rafael G. Lund

  3. Dental Materials Laboratory, Academic Area of Dentistry, Autonomous University of Hidalgo State, Circuito Ex Hacienda La Concepción S/N, 42160, San Agustín Tlaxiaca, Hidalgo, Mexico

    Carlos E. Cuevas Suárez

  4. Department of Biomedical Engineering, College of Engineering, University of Michigan, Ann Arbor, MI, USA

    Marco C. Bottino

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  1. Juliana S. Ribeiro
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  2. Samantha R. Xavier
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Contributions

All authors have read and approved the manuscript. Conceptualization: Xavier SR, Ribeiro JS. Data curation: Ribeiro JS, Xavier SR, Suárez CEC, Pappen FG. Formal analysis: Ribeiro JS, Xavier SR, Suárez CEC. Investigation: Ribeiro JS, Xavier SR, Suárez CEC. Methodology: Ribeiro JS, Xavier SR, Suárez CEC. Project administration: Ribeiro JS. Resources: Piva E, Lund RG, Bottino MC. Supervision: Lund RG, Bottino MC. Validation: Ribeiro JS. Visualization: Ribeiro JS, Pappen FG, Piva E. Writing—original draft: Ribeiro JS, Xavier SR, Suárez CEC. Writing—review and editing: Ribeiro JS, Lund RG, Bottino MC.

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Correspondence to Marco C. Bottino.

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Ribeiro, J.S., Xavier, S.R., Cuevas Suárez, C.E. et al. Synthesis and characterization of calcium-releasing elastomeric resin-based endodontic sealers. Clin Oral Invest 27, 3447–3456 (2023). https://doi.org/10.1007/s00784-023-04952-0

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