Development and application of calcium phosphate particles functionalized with acidic monomers for dental remineralization

The aims of this study were: 1) to synthesize and characterize dicalcium phosphate dihydrate (DCPD) particles functionalized with different organic agents (citric acid/CA, acrylic acid/AA, methacryloyloxyethyl phosphate/MOEP and diethylene glycol dimethacrylate/DEGDMA) and 2) evaluate the effect of the addition of these particles over physical-chemical properties and remineralization potential of experimental composites. In the first part of the study, DCPD particles were synthesized by a coprecipitation method in the presence of citric acid, acrylic acid, MOEP, DEGDMA or without functionalizing agent (non-functionalized/NF). Particles were characterized by X-ray diffraction (XRD), elemental analysis, density, surface area, laser diffraction, scanning electron microscopy (SEM) and zeta potential. In the second part, six resinbased materials were manipulated, containing in the organic phase bisphenol A glycerolate dimethacrylate (BisGMA)/triethylene glycol dimethacrylate (TEGDMA) (1:1 in mols), photoiniciators and 60 vol% of particles, composed by silanized barium glass and 0% (control: without DCPD) or 20 vol% of DCPD particles. Materials were evaluated for degree of conversion (DC), biaxial flexural strength (BFS) and flexural modulus (E) after 24 hours and 60 days of immersion in water, ion release and protective effect on adjacent enamel submitted to an in vitro cariogenic challenge. Data from DC, E, ion release ?KHNsurface/?KHNcross-sectional were subjected to analysis of variance (ANOVA)/Tukey test. Data from BFS were analyzed using Kruskal- Wallis/Dunn test. In all cases, the global significance level was 5%. DCPD formation was confirmed by XRD. Elemental analysis presented the retention of functionalizing agent retention at levels above 1.5% only for DCPD-DEGDMA, which also had reduction in density due to the presence of the functionalizing monomer. Surface area measurements were similar for all particles (22 - 30 m2/g). Particles synthesized in the presence of citric acid presented smaller size in relation to the others. Zeta potential values ranged from -0.9 to -14.2 mV. All composites presented similar DC. For BFS, after 24 hours, only the materials containing DCPD-AA and DCPDDEGDMA were statistically similar to the control, but after prolonged immersion only the material containing DCPD-DEGDMA remained statistically similar to the control. For E, after 24 hours, the composites containing DCPD-NF, DCPD-MOEP, DCPDDEGDMA or DCPD-AA were statistically similar and presented higher results than the control. After immersion, all composites were similar to the control, except for DCPD-AA, which had lower results. The material containing DCPD-CA presented higher ionic releases than the DCPD-DEGDMA, this possibly reflected on the lower results for ?KHNsurface for the specimens restored with the composite containing DCPD-CA in comparison to DCPD-DEGDMA material. For ?KHNcross-sectional, there was no statistically significant interaction for the factors. The highest reductions were observed at 10 ?m and 30 ?m dephts. Also, the enamel around the composite containing DCPD-AA presented higher reduction in KHN than the materials containing DCPD-NF and than the control. DCPD synthesis was successful. However, only citric acid was effective to reduce particle size. DEGDMA was the functionalizing agent that presented higher levels of retention in the particle surface. In addition, functionalization with DEGDMA favored the interaction between DCPD and the organic matrix, evidenced by the higher resuts of flexural strength. However ion release was compromised. In 7 days the DCPD-containing composites did not prersented a protective effect against the demineralization caused by the pH cycling. (AU)