Correlative micro-Raman/EPMA analysis of the hydraulic calcium silicate cement interface with dentin

Objectives: This study aims to characterize the chemical interplay of hydraulic calcium silicate cements at dentin.

Materials and methods: Class I cavities were prepared in non-carious human third molars and filled with Biodentine (Septodont) or ProRoot MTA (Dentsply). After 1-day, 1-week, and 1-month Dulbecco's phosphate-buffered saline (DPBS) storage, the specimens were cross-sectioned perpendicular to the cement-dentin interface. The interfaces were evaluated using micro-Raman (μRaman) spectroscopy and at a higher spatial resolution using field emission gun electron probe microanalysis (Feg-SEM/EPMA).

Results: μRaman spectroscopy revealed the formation of a transition zone at the interface of both Biodentine (Septodont) and ProRoot MTA (Dentsply) with dentin, having an average thickness of, respectively, 7.5 ± 4.2 and 6.2 ± 5.4 μm, which however was not statistically different. No difference in interfacial ultrastructure and chemistry was found using μRaman spectroscopy between 1 day, 1 week, and 1 month DPBS-stored specimens. The observation of a transition zone at the cement-dentin interfaces contrasts with the EPMA data that revealed a sharper transition from cement to dentin. Again, no difference in interfacial ultrastructure and chemistry was found for different storage periods, with the exception of one 1 month DPBS-stored specimen prepared using Biodentine (Septodont). More specifically, EPMA revealed a gap of about 10-μm wide in the latter specimen that was filled up with newly formed calcium phosphate depositions.

Conclusions: Up to 1 month, the interaction of hydraulic calcium silicate cements investigated did not reveal ultrastructural or chemical changes at unaffected dentin with the exception of a calcium phosphate gap-filling property.

Clinical relevance: Hydraulic calcium silicate cements were found to fill gaps by calcium phosphate deposition, however, without conducting chemical changes to the adjacent dentin.