Experimental dentin adhesives containing calcium orthophosphate particles: Effect on dentin bond strength, micro-permeability and collagen degradation

To assess the effect of dicalcium phosphate dihydrate (DCPD) or mineral trioxide aggregate (MTA) particles on the microtensile bond strength (μTBS), micro-permeability and enzymatic activity at the adhesive-dentin interface of experimental dental adhesives. An experimental ethanol-based, two-step etch-and-rinse adhesive system was prepared. Four experimental groups were tested, based on the type of particle added: (1) DCPD functionalized with diethylene glycol dimethacrylate (DCPD_DEGDMA), (2) citric acid (DCPD_CA), (3) calcium silicate (MTA) and (4) unfilled (control). All particles were added at 10 wt%. Human third molars had their occlusal enamel removed and dentin surface polished. After acid etching, the adhesives were applied on the dentin surfaces and the teeth were restored with a commercial nanofilled resin composite. The μTBS and micro-permeability were tested after 24 h or 2 months of storage in simulated body fluid (SBF) at 37 °C. Bonded interfaces were observed using scanning electron microcopy (SEM). Gelatinolytic activity at the adhesive interfaces was assessed by in situ zymography at 24 h and 2 months in SBF/37 °C. The results were described as relative florescent units (RFU). μTBS data were analyzed by ANOVA/Games–Howell test. Data from micro-permeability and in situ zymography were analyzed by Kruskal–Wallis/Mann–Whitney test (alpha: 5%). Differences in μTBS were found among adhesives (control = MTA > DCPD_CA > DCPD_DEGDMA, p