Preparation and characterization properties of three different ratios of biphasic calcium phosphate

doi:10.12307/2026.604

Abstract

Abstract: BACKGROUND: Root canal sealers, which are widely used in current clinical practice, still have the disadvantages of poor biocompatibility and poor degradability.
OBJECTIVE: To prepare nanohydroxyapatite and β-tricalcium phosphate biphasic calcium phosphate composites with polyvinyl alcohol as the binder and characterize the properties of the composites.
METHODS: 15% polyvinyl alcohol hydrogel was mixed with different proportions of nanohydroxyapatite and β-tricalcium phosphate (the mass ratio of nanohydroxyapatite to β-tricalcium phosphate was 30:70, 40:60, and 50:50, respectively). Biphasic calcium phosphate/polyvinyl alcohol composites were prepared by freeze drying. 30% nanohydroxyapatite/polyvinyl alcohol composites and 30% β-tricalcium phosphate/polyvinyl alcohol composites were prepared at the same time. Scanning electron microscope, X-ray energy dispersive spectroscopy, X-ray diffractometer, X-ray photoelectron spectroscopy, and Fourier infrared spectroscopy were used to characterize the physical and chemical properties of each group of composites. The mechanical properties of each group of composites were studied by universal mechanical testing machine.
RESULTS AND CONCLUSION: (1) Scanning electron microscopy and X-ray energy dispersive spectroscopy showed that nanohydroxyapatite and β-tricalcium phosphate in the biphasic calcium phosphate/polyvinyl alcohol composites were clustered together, and the C, O, Ca, and P elements were evenly distributed. (2) X-ray diffraction, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy results of the biphasic calcium phosphate/polyvinyl alcohol composites showed that polyvinyl alcohol was successfully mixed with nanohydroxyapatite and β-tricalcium phosphate without chemical structure changes. (3) There were no significant differences in the ultimate compressive strength and elastic modulus of the five groups of composites (P > 0.05), among which the elastic modulus of the biphasic calcium phosphate (40:60)/polyvinyl alcohol composite was the largest.

Key words: biphasic calcium phosphate, hydroxyapatite, β-tricalcium phosphate, polyvinyl alcohol, root canal sealer, mechanical property

CLC Number:

Shao Ziyu, Li Qian, Qumanguli·Abudukelimu, Han Youjun, Hu Yang. Preparation and characterization properties of three different ratios of biphasic calcium phosphate[J]. Chinese Journal of Tissue Engineering Research, 2026, 30(8): 1952-1961.

Figures/Tables 11

References

[1] DEVI MT, SAHA S, TRIPATHI AM, et al. Evaluation of the Antimicrobial Efficacy of Herbal Extracts Added to Root Canal Sealers of Different Bases: An In Vitro Study. Int J Clin Pediatr Dent. 2019;12(5):398-404.
[2] BUURMA HA, BUURMA BJ. The effect of smear layer on bacterial penetration through roots obturated using zinc oxide eugenol-based sealer. BMC Oral Health. 2020;20(1):88.
[3] KHANDELWAL A, JOSE J, TEJA K, et al. Comparative evaluation of postoperative pain and periapical healing after root canal treatment using three different base endodontic sealers - A randomized control clinical trial. J Clin Exp Dent. 2022;14(2):e144-e152.
[4] Alvarez-Vasquez JL, Erazo-Guijarro MJ, Dominguez-Ordonez GS, et al. Epoxy resin-based root canal sealers: An integrative literature review. Dent Med Probl. 2024;61(2):279-291.
[5] ORTEGA MA, RIOS L, FRAILE-MARTINEZ O, et al. Bioceramic versus traditional biomaterials for endodontic sealers according to the ideal properties. Histol Histopathol. 2024;39(3):279-292.
[6] SONG W, SUN W, CHEN L, et al. In vivo Biocompatibility and Bioactivity of Calcium Silicate-Based Bioceramics in Endodontics. Front Bioeng Biotechnol. 2020;8:580954.
[7] BAE WJ, Chang SW, Lee SI, et al. Human periodontal ligament cell response to a newly developed calcium phosphate-based root canal sealer. J Endod. 2010;36(10):1658-1663.
[8] VICTOR SP, KUMAR TS. BCP ceramic microspheres as drug delivery carriers: synthesis, characterisation and doxycycline release. J Mater Sci Mater Med. 2008;19(1):283-290.
[9] DA SILVA BRUM I, FRIGO L, GONCALO PINTO DOS SANTOS P, et al. Performance of Nano-Hydroxyapatite/Beta-Tricalcium Phosphate and Xenogenic Hydroxyapatite on Bone Regeneration in Rat Calvarial Defects: Histomorphometric, Immunohistochemical and Ultrastructural Analysis. Int J Nanomedicine. 2021;16:3473-3485.
[10] ZARKESH I, GHANIAN MH, AZAMI M, et al. Facile synthesis of biphasic calcium phosphate microspheres with engineered surface topography for controlled delivery of drugs and proteins. Colloids Surf B Biointerfaces. 2017;157:223-232.
[11] ZHONG Y, LIN Q, YU H, et al. Construction methods and biomedical applications of PVA-based hydrogels. Front Chem. 2024;12:1376799.
[12] SAITO H, COUSO-QUEIRUGA E, SHIAU HJ, et al. Evaluation of poly lactic‐co‐glycolic acid‐coated β‐tricalcium phosphate for alveolar ridge preservation: A multicenter randomized controlled trial. J Periodontol. 2021;92(4):524-535.
[13] HUI H, SONG Y, LIU H, et al. Integrating molecular-caged nano-hydroxyapatite into post-crosslinked PVA nanofibers for artificial periosteum. Biomater Adv. 2024;165:214001.
[14] RAY HA, TROPE M. Periapical status of endodontically treated teeth in relation to the technical quality of the root filling and the coronal restoration. Int Endod J. 1995;28(1):12-18.
[15] WANG X, XIAO Y, SONG W, et al. Clinical application of calcium silicate-based bioceramics in endodontics. J Transl Med. 2023;21(1):853.
[16] AL-HADDAD A, CHE AB AZIZ ZA. Bioceramic-Based Root Canal Sealers: A Review. Int J Biomater. 2016;2016:9753210.
[17] ULANOWSKA M, OLAS B. Biological Properties and Prospects for the Application of Eugenol-A Review. Int J Mol Sci. 2021;22(7):3671.
[18] VERTUAN GC, DUARTE MAH, MORAES IG, et al. Evaluation of Physicochemical Properties of a New Root Canal Sealer. J Endod. 2018;44(3):501-505.
[19] DONNERMEYER D, BURKLEIN S, DAMMASCHKE T, et al. Endodontic sealers based on calcium silicates: a systematic review. Odontology. 2019;107(4):421-436.
[20] MCMICHEN FR, PEARSON G, RAHBARAN S, et al. A comparative study of selected physical properties of five root-canal sealers. Int Endod J. 2003;36(9):629-635.
[21] LU H, LU J, GUO J, et al. Radiographic outcomes and prognostic factors in nonvital immature permanent teeth after apexification with modified calcium hydroxide paste: a retrospective study. Clin Oral Investig. 2022;26(7):5079-5088.
[22] KANG Q, HUANG Z, QIAN W. Nicolau Syndrome with Severe Facial Ischemic Necrosis after Endodontic Treatment: A Case Report. J Endod. 2024;50(5):680-686.
[23] AL-SHEEB F, AL MANNAI G, THARUPEEDIKAYIL S. Nicolau Syndrome after Endodontic Treatment: A Case Report. J Endod. 2022;48(2): 269-272.
[24] CHEAH CW, AL-NAMNAM NM, LAU MN, et al. Synthetic Material for Bone, Periodontal, and Dental Tissue Regeneration: Where Are We Now, and Where Are We Heading Next? Materials (Basel). 2021; 14(20):6123.
[25] LEGEROS RZ, LIN S, ROHANIZADEH R, et al. Biphasic calcium phosphate bioceramics: preparation, properties and applications. J Mater Sci Mater Med. 2003;14(3):201-209.
[26] BROWN O, MCAFEE M, CLARKE S, et al. Sintering of biphasic calcium phosphates. J Mater Sci Mater Med. 2010;21(8):2271-2279.
[27] EBRAHIMI M, PRIPATNANONT P, MONMATURAPOJ N, et al. Fabrication and characterization of novel nano hydroxyapatite/beta-tricalcium phosphate scaffolds in three different composition ratios. J Biomed Mater Res A. 2012;100(9):2260-2268.
[28] MANDATORI D, D’AMICO E, ROMASCO T, et al. A 3D in vitro model of biphasic calcium phosphate (BCP) scaffold combined with human osteoblasts, osteoclasts, and endothelial cells as a platform to mimic the oral microenvironment for tissue regeneration. J Dent. 2024;151:105411.
[29] ZHANG K, LIU Y, ZHAO Z, et al. Magnesium-Doped Nano-Hydroxyapatite/Polyvinyl Alcohol/Chitosan Composite Hydrogel: Preparation and Characterization. Int J Nanomedicine. 2024;19:
651-671.
[30] YANG G, LIU X, HUANG T, et al. Combined Application of Dentin Noncollagenous Proteins and Odontogenic Biphasic Calcium Phosphate in Rabbit Maxillary Sinus Lifting. Tissue Eng Regen Med. 2023;20(1): 93-109.
[31] RUJIRAPRASERT P, SURIYASANGPETCH S, SRIJUNBARL A, et al. Calcium phosphate ceramic as a model for enamel substitute material in dental applications. BDJ Open. 2023;9(1):25.
[32] MANSOUR AM, ABOU HAMMAD AB, EL NAHRAWY AM. Exploring nanoarchitectonics and optical properties of PAA-ZnO@BCP wide-band-gap organic semiconductors. Sci Rep. 2024;14(1):3060.
[33] FRANCA R, SAMANI TD, BAYADE G, et al. Nanoscale surface characterization of biphasic calcium phosphate, with comparisons to calcium hydroxyapatite and beta-tricalcium phosphate bioceramics. J Colloid Interface Sci. 2014;420:182-188.
[34] SOARES I, SOTELO L, ERCEG I, et al. Improvement of Metal-Doped beta-TCP Scaffolds for Active Bone Substitutes via Ultra-Short Laser Structuring. Bioengineering (Basel). 2023;10(12):1392.
[35] THUAKSUBAN N, LUNTHENG T, MONMATURAPOJ N. Physical characteristics and biocompatibility of the polycaprolactone-biphasic calcium phosphate scaffolds fabricated using the modified melt stretching and multilayer deposition. J Biomater Appl. 2016; 30(10):1460-1472.
[36] GU Y, BAI Y, ZHANG D. Osteogenic stimulation of human dental pulp stem cells with a novel gelatin‐hydroxyapatite‐tricalcium phosphate scaffold. J Biomed Mater Res A. 2018;106(7):1851-1861.