Apatite-like calcium phosphate deposition and physicochemical properties of an aspartic acid–functionalized hydraulic cement

Abstract Objectives This study evaluated the effects of aspartic acid modification on the physicochemical properties and phosphate-associated surface response of a hydraulic calcium silicate cement. Materials and methods White mineral trioxide aggregate (MTA) was mixed using 0%, 25%, 50%, 75%, or 100% (v/v) of a 4 g/L aspartic acid stock solution. Final setting time, solubility, pH, and Ca²⁺ concentration in the immersion solution were evaluated after seven days in deionized water ( n = 10). Surface roughness, morphology, elemental composition, and phosphate- and carbonate-associated spectral features were assessed after 30 days of storage in deionized water or phosphate-buffered saline (PBS). The Ap/C spectral ratio was calculated from the integrated ATR-FTIR band areas. Data were analyzed using one- or two-way ANOVA followed by Tukey’s test (α = 0.05). Results The 25% formulation showed the shortest setting time, whereas the 100% formulation showed the longest ( p < 0.001). All aspartic acid-containing formulations exhibited greater solubility and lower Ca²⁺ concentrations than the control ( p < 0.05), and the 50%, 75%, and 100% formulations exceeded the recommended solubility limit. The 25% formulation had the lowest pH, whereas the control, 75%, and 100% formulations maintained similar alkaline values. Surface roughness was lowest for the 25% formulation and highest for the 100% formulation, with no significant effect of storage medium. EDS detected negligible surface phosphorus after storage in deionized water but marked phosphorus content after PBS storage. Ap/C analysis showed significant main effects of cement formulation and storage medium, without a significant interaction. The 25%, 50%, and 75% formulations exhibited higher marginal Ap/C ratios than the 0% and 100% formulations. Conclusions Aspartic acid produced non-linear and formulation-dependent changes in the evaluated properties. Higher Ap/C ratios reflected differences in relative spectral composition but did not confirm increased apatite formation or a crystalline apatite phase. Ca–P-rich surface deposition depended on phosphate supplied by the storage medium, and no formulation improved all evaluated outcomes.

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Publication Details

Journal
Clinical Oral Investigations
Published
2026-10-03
DOI
https://doi.org/10.1007/s00784-026-07196-w
Primary Topic
Endodontics and Root Canal Treatments
Type
article
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article

Apatite-like calcium phosphate deposition and physicochemical properties of an aspartic acid–functionalized hydraulic cement

Larissa Moreira Spinola de Castro Raucci, Elias Daniel Covas Rodrigues, Marcelle Danelon, Walter Raucci Neto et al.
Clinical Oral Investigations
Endodontics and Root Canal Treatments
article

Apatite-like calcium phosphate deposition and physicochemical properties of an aspartic acid–functionalized hydraulic cement

Larissa Moreira Spinola de Castro Raucci, Elias Daniel Covas Rodrigues, Marcelle Danelon, Walter Raucci Neto, Regina Guenka Palma‐Dibb, Victor Miguel Polizeli, Larissa Fernanda Pereira, Júlia Tavares de Sousa
article en

Abstract

Abstract Objectives This study evaluated the effects of aspartic acid modification on the physicochemical properties and phosphate-associated surface response of a hydraulic calcium silicate cement. Materials and methods White mineral trioxide aggregate (MTA) was mixed using 0%, 25%, 50%, 75%, or 100% (v/v) of a 4 g/L aspartic acid stock solution. Final setting time, solubility, pH, and Ca²⁺ concentration in the immersion solution were evaluated after seven days in deionized water ( n = 10). Surface roughness, morphology, elemental composition, and phosphate- and carbonate-associated spectral features were assessed after 30 days of storage in deionized water or phosphate-buffered saline (PBS). The Ap/C spectral ratio was calculated from the integrated ATR-FTIR band areas. Data were analyzed using one- or two-way ANOVA followed by Tukey’s test (α = 0.05). Results The 25% formulation showed the shortest setting time, whereas the 100% formulation showed the longest ( p < 0.001). All aspartic acid-containing formulations exhibited greater solubility and lower Ca²⁺ concentrations than the control ( p < 0.05), and the 50%, 75%, and 100% formulations exceeded the recommended solubility limit. The 25% formulation had the lowest pH, whereas the control, 75%, and 100% formulations maintained similar alkaline values. Surface roughness was lowest for the 25% formulation and highest for the 100% formulation, with no significant effect of storage medium. EDS detected negligible surface phosphorus after storage in deionized water but marked phosphorus content after PBS storage. Ap/C analysis showed significant main effects of cement formulation and storage medium, without a significant interaction. The 25%, 50%, and 75% formulations exhibited higher marginal Ap/C ratios than the 0% and 100% formulations. Conclusions Aspartic acid produced non-linear and formulation-dependent changes in the evaluated properties. Higher Ap/C ratios reflected differences in relative spectral composition but did not confirm increased apatite formation or a crystalline apatite phase. Ca–P-rich surface deposition depended on phosphate supplied by the storage medium, and no formulation improved all evaluated outcomes.

Clinical Oral InvestigationsVol. 30(10)
Universidade de Ribeirão Preto (BR), University Hospital Carl Gustav Carus (DE)
Openalex Percentile: Top 9%
Endodontics and Root Canal Treatments
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