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

Xin Li; Pong Pongprueksa; Kirsten Van Landuyt; Zhi Chen; Mariano Pedano; Bart Van Meerbeek; Jan De Munck

doi:10.1007/s00784-015-1650-x

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

Clin Oral Investig. 2016 Sep;20(7):1663-73. doi: 10.1007/s00784-015-1650-x. Epub 2015 Nov 10.

Authors

Xin Li^{1

2}, Pong Pongprueksa¹, Kirsten Van Landuyt¹, Zhi Chen², Mariano Pedano¹, Bart Van Meerbeek³, Jan De Munck¹

Affiliations

¹ BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven) & Dentistry, University Hospitals Leuven, Kapucijnenvoer 7, blok A - box 7001, Leuven, BE-3000, Belgium.
² The State Key Laboratory Breeding Base of Basic Science of Stomatology (Hubei-MOST) & Key Laboratory of Oral Biomedicine Ministry of Education, School and Hospital of Stomatology, Wuhan University, Wuhan, PR, China.
³ BIOMAT, Department of Oral Health Sciences, KU Leuven (University of Leuven) & Dentistry, University Hospitals Leuven, Kapucijnenvoer 7, blok A - box 7001, Leuven, BE-3000, Belgium. bart.vanmeerbeek@med.kuleuven.be.

PMID: 26556572
DOI: 10.1007/s00784-015-1650-x

Abstract

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.

Keywords: EPMA; Hydraulic calcium silicate cement; Interfacial interaction; Micro-Raman spectroscopy.

MeSH terms

Aluminum Compounds / chemistry*
Calcium Compounds / chemistry*
Dental Cements / chemistry*
Dentin / drug effects*
Dentin / ultrastructure*
Drug Combinations
Electron Probe Microanalysis
Humans
In Vitro Techniques
Molar, Third
Oxides / chemistry*
Silicate Cement / chemistry*
Silicates / chemistry*
Spectrum Analysis, Raman

Substances

Aluminum Compounds
Calcium Compounds
Dental Cements
Drug Combinations
Oxides
Silicates
mineral trioxide aggregate
Silicate Cement
tricalcium silicate