Effect of borate, fluoride and strontium ions on biomimetic nucleation of calcium phosphate studied using solid-state nuclear magnetic resonance and X-ray diffraction.

OBJECTIVES: Apatite minerals can have various anions and cations in their crystal structure in addition to phosphate ion (PO4³â») and calcium ion (Ca2+). The aim of this study is to investigate effects of the borate, fluoride and strontium ions on biomimetic nucleation of calcium phosphate. METHODS: Nano-crystalline hydroxyapatite (H-Ap) was obtained from a supersaturated buffered solution containing 4.12 mM HPO42- and 5.88 mM Ca2+ (H-Ap). Four additives were used in solid solution methods: (i) 0.588 mM F- (F-Ap), (ii) 5.88 mM Sr2+ (Sr-Ap), (iii) 4.12 mM BO33- (BO3-Ap), and (iv) a surface pre-reacted glass ionomer (S-PRG) filler eluate that contained 0.17 mM Sr2+, 0.588 mM F-, 11.1 mM BO33-- (SPRG-Ap). Apatite crystallization was investigated using a solid-state magic-angle spinning NMR spectroscopy and X-ray diffraction (XRD) with the Rietveld analysis. RESULTS: A 2D 1H-31P heteronuclear-correlation NMR showed F- ion incorporation in the apatite structure of the F-Ap and SPRG-Ap. The peaks on the 31P axis of the F-Ap, Sr-Ap, and BO3-Ap were different from that of the H-Ap, and the full width at half maximum increased in the following order: H-Ap∼F-Ap∼BO3-Ap< SPRG-Ap< Sr-Ap, suggesting the incorporation of the F-, Sr2+ and BO33-. The incorporation of F and BO3 was further confirmed by 19F and 11B NMR. The XRD revealed that Sr2+ was preferentially incorporated into the CaII site. SIGNIFICANCE: The F-, Sr2+ and BO33-ions might be involved in modifying the crystallization of apatite precipitation, producing a variety of apatite. S-PRG filler that release these ions may have an effect on remineralization, i.e., the reformation of apatite lost due to caries.

Crystallographic and Physicochemical Analysis of Bovine and Human Teeth Using X-ray Diffraction and Solid-State Nuclear Magnetic Resonance.

Dental research often uses bovine teeth as a substitute for human teeth. The aim of this study was to evaluate differences in the crystalline nanostructures of enamel and dentin between bovine and human teeth, using X-ray diffraction (XRD) and solid-state nuclear magnetic resonance (NMR). The crystallite size (crystallinity) and microstrains were analyzed using XRD with the Rietveld refinement technique and the Halder-Wagner method. The 31P and 1H NMR chemical environments were analyzed by two-dimensional (2D) 1H-31P heteronuclear-correlation (HETCOR) magic-angle spinning (MAS) NMR spectroscopy. Enamel had a greater crystallite size and fewer microstrains than dentin for both bovine and human teeth. When compared between the species, the bovine apatite had a smaller crystallite size with more microstrains than the human apatite for both dentin and enamel. The 2D HETCOR spectra demonstrated that a water-rich layer and inorganic HPO4- ions were abundant in dentin; meanwhile, the hydroxyl group in the lattice site was more dominant in enamel. A greater intensity of the hydroxyl group was detected in human than in bovine for both dentin and enamel. For 31P projections, bovine dentin and bovine enamel have wider linewidths than human dentin and human enamel, respectively. There are differences in the crystallite profile between human and bovine. The results of dental research should be interpreted with caution when bovine teeth are substituted for human teeth.

Evaluation of Incipient Enamel Caries at Smooth Tooth Surfaces Using SS-OCT.

(1) Background: Dental caries, if diagnosed at the initial stage, can be arrested and remineralized by a non-operative therapeutic approach preserving tooth structure. Accurate and reproducible diagnostic procedure is required for the successful management of incipient caries. The aim of this study was to evaluate the diagnostic accuracy of 3D swept-source optical coherence tomography (3D SS-OCT) for enamel caries at smooth tooth surface if the lesion was with remineralization. (2) Methods: Forty-seven tooth surfaces of 24 extracted human teeth visibly with/without enamel caries (ICDAS code 0−3) were selected and used in this study. The tooth surfaces of investigation site were cleaned and visually examined by four dentists. After the visual inspection, SS-OCT scanning was performed onto the enamel surfaces to construct a 3D image. The 2D tomographic images of the investigation site were chosen from the 3D dataset and dynamically displayed in video and evaluated by the examiners. A five-rank scale was used to score the level of enamel caries according to the following; 1: Intact enamel. 2: Noncavitated lesion with remineralization. 3: Superficial noncavitated lesion without remineralization. 4: Deep nonvacitated lesion without remineralization. 5: Enamel lesion with cavitation. Sensitivity and specificity for 3D OCT image and visual inspection were calculated. Diagnostic accuracy of each diagnostic method was calculated using weighted kappa. Statistical significance was defined at p = 0.05. (3) Results: 3D SS-OCT could clearly depict enamel caries at smooth tooth surface as a bright zone, based on the increased backscattering signal. It was noted that 3D SS-OCT showed higher sensitivity for the diagnosis of remineralized lesions and deep enamel lesions without cavitation, as well as cavitated enamel lesions (p < 0.05). No significant difference of specificity was observed between the two diagnostic methods (p > 0.05). Furthermore, 3D SS-OCT showed higher diagnostic accuracy than visual inspection (p < 0.05). (4) Conclusions: Within the limitations of this in vitro study, 3D SS-OCT showed higher diagnostic capacity for smooth surface enamel caries than visual inspection and could also discriminate lesion remineralization of enamel caries.