RESUMO
OBJECTIVE: To investigate the effects of natural collagen cross-linkers incorporation in phosphoric acid etchant on dentin biomodification, microtensile bond strength (µTBS) and nanoleakage (NL) of a two-step etch-and-rinse adhesive. METHODS: Experimental aqueous solution of 37% ortho-phosphoric acid were prepared with the addition of 2% biomodification agents: Lignin (LIG) from industrial paper production residue, Cardanol (CARD) from cashew-nut shell liquid, and Proanthocyanidin (PAC) from grape-seed extract. Negative control (NC) was acid solution without cross-linker whilst commercial control (CC) was Condac 37 gel (FGM). Dentin specimens were assayed by FTIR after 15s etching to detect collagen cross-linking. Extracted third molars were used for µTBS (n=7) and fracture mode analysis of Optibond S (Kerr), tested after 24h or 1000 thermal cycles. NL was surveyed by SEM. Statistical analysis was performed with two-way ANOVA and Tukey's test (p<0.05). RESULTS: FTIR confirmed cross-linking for all agents. µTBS of CC was the highest (46.6±6.2MPa), but reduced significantly after aging (35.7±5.2MPa) (p<0.001). LIG (30.6±3.7MPa) and CARD (28.3±1.8MPa) attained similar µTBS which were stable after aging (p>0.05). Fracture mode was predominantly adhesive. At 24h, all groups showed presence of silver uptake in hybrid layer, except CARD. After aging, CARD- and LIG-treated specimens exhibited little amount of silver penetration. CC, PAC and NC showed gaps, great nanoleakage at hybrid layer and presence of water channels in adhesive layer. SIGNIFICANCE: Altogether, ortho-phosphoric acid incorporated with LIG and CARD promotes stable resin-dentin bond strength with minor nanoleakage after aging, thereby achieving therapeutic impact without additional clinical steps.