Chlorhexidine-modified nanotubes and their effects on the polymerization and bonding performance of a dental adhesive.

OBJECTIVES: The purpose of this study was to synthesize chlorhexidine (CHX)-encapsulated aluminosilicate clay nanotubes (Halloysite®, HNTs) and to incorporate them into the primer/adhesive components of an etch-and-rinse adhesive system (SBMP; Scotchbond Multipurpose, 3M ESPE) and to test their effects on degree of conversion, viscosity, immediate and long-term bonding to dentin. METHODS: CHX-modified HNTs were synthesized using 10% or 20% CHX solutions. The primer and the adhesive components of SBMP were incorporated with 15wt.% of the CHX-encapsulated HNTs. Degree of conversion (DC) and viscosity analyses were performed to characterize the modified primers/adhesives. For bond strength testing, acid-etched dentin was treated with one of the following: SBMP (control); 0.2%CHX solution before SBMP; CHX-modified primers+SBMP adhesive; SBMP primer+CHX-modified adhesives; and SBMP primer+CHX-free HNT-modified adhesive. The microtensile bond strength test was performed after immediate (24h) and long-term (6 months) of water storage. Data were analyzed using ANOVA and Tukey (α=5%) and the Weibull analysis. RESULTS: DC was greater for the CHX-free HNT-modified adhesive, whereas the other experimental adhesives showed similar DC as compared with the control. Primers were less viscous than the adhesives, without significant differences within the respective materials. At 24h, all groups showed similar bonding performance and structural reliability; whereas at the 6-month period, groups treated with the 0.2%CHX solution prior bonding or with the CHX-modified primers resulted in greater bond strength than the control and superior reliability. SIGNIFICANCE: The modification of a primer or adhesive with CHX-encapsulated HNTs was an advantageous approach that did not impair the polymerization, viscosity and bonding performance of the materials, showing a promising long-term effect on resin-dentin bonds.

Physicochemical and biological properties of novel chlorhexidine-loaded nanotube-modified dentin adhesive.

A commercially available three-step (etch-and-rinse) adhesive was modified by adding chlorhexidine (CHX)-loaded nanotubes (Halloysite®, HNT) at two concentrations (CHX10% and CHX20%). The experimental groups were: SBMP (unmodified adhesive, control), HNT (SBMP modified with HNT), CHX10 (SBMP modified with HNT loaded with CHX10%), and CHX20 (SBMP modified with HNT loaded with CHX20%). Changes in the degree of conversion (DC%), Knoop hardness (KHN), water sorption (WS), solubility (SL), antimicrobial activity, cytotoxicity, and anti-matrix metalloproteinase [MMP-1] activity (collagenase-I) were evaluated. In regards to DC%, two-way ANOVA followed by Tukey's post-hoc test revealed that only the factor "adhesive" was statistically significant (p < 0.05). No significant differences were detected in DC% when 20 s light-curing was used (p > 0.05). For Knoop microhardness, one-way ANOVA followed by the Tukey's test showed statistically significant differences when comparing HNT (20.82 ± 1.65) and CHX20% (21.71 ± 2.83) with the SBMP and CHX10% groups. All adhesives presented similar WS and cytocompatibility. The CHX-loaded nanotube-modified adhesive released enough CHX to inhibit the growth of S. mutans and L. casei. Adhesive eluates were not able to effectively inhibit MMP-1 activity. The evaluation of higher CHX concentrations might be necessary to provide an effective and predictable MMP inhibition. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res B Part B, 2018. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater 107B: 868-875, 2019.

Clindamycin-modified Triple Antibiotic Nanofibers: A Stain-free Antimicrobial Intracanal Drug Delivery System.

INTRODUCTION: A biocompatible strategy to promote bacterial eradication within the root canal system after pulpal necrosis of immature permanent teeth is critical to the success of regenerative endodontic procedures. This study sought to synthesize clindamycin-modified triple antibiotic (metronidazole, ciprofloxacin, and clindamycin [CLIN]) polymer (polydioxanone [PDS]) nanofibers and determine in vitro their antimicrobial properties, cell compatibility, and dentin discoloration. METHODS: CLIN-only and triple antibiotic CLIN-modified (CLIN-m, minocycline-free) nanofibers were processed via electrospinning. Scanning electron microscopy, Fourier-transform infrared spectroscopy (FTIR), and tensile testing were performed to investigate fiber morphology, antibiotic incorporation, and mechanical strength, respectively. Antimicrobial properties of CLIN-only and CLIN-m nanofibers were assessed against several bacterial species by direct nanofiber/bacteria contact and over time based on aliquot collection up to 21 days. Cytocompatibility was measured against human dental pulp stem cells. Dentin discoloration upon nanofiber exposure was qualitatively recorded over time. The data were statistically analyzed (P < .05). RESULTS: The mean fiber diameter of CLIN-containing nanofibers ranged between 352 ± 128 nm and 349 ± 128 nm and was significantly smaller than PDS fibers. FTIR analysis confirmed the presence of antibiotics in the nanofibers. Hydrated CLIN-m nanofibers showed similar tensile strength to antibiotic-free (PDS) nanofibers. All CLIN-containing nanofibers and aliquots demonstrated pronounced antimicrobial activity against all bacteria. Antibiotic-containing aliquots led to a slight reduction in dental pulp stem cell viability but were not considered toxic. No visible dentin discoloration upon CLIN-containing nanofiber exposure was observed. CONCLUSIONS: Collectively, based on the remarkable antimicrobial effects, cell-friendly, and stain-free properties, our data suggest that CLIN-m triple antibiotic nanofibers might be a viable alternative to minocycline-based antibiotic pastes.

Synthesis and characterization of novel halloysite-incorporated adhesive resins.

OBJECTIVE: To investigate the effects of Halloysite® aluminosilicate clay nanotubes (HNTs) addition on selected physical, mechanical, and biological properties of experimental adhesive resins. METHODS: Experimental dentin adhesive resins were prepared by mixing Bis-GMA, TEGDMA, HEMA (50/25/25wt.%), and photo-initiators. As-received HNTs were then incorporated into the resin mixture at distinct concentrations: 0 (HNT-free, control), 1, 2.5, 5, 7.5, 10, and 20wt.%. The degree of conversion (DC), radiopacity (RP), Knoop hardness (KHN), flexural strength (FS), and cytotoxicity analyses were carried out for each adhesive formulation. The adhesive resin of Adper Scotchbond Multi-Purpose (SBMP) was used as the commercially available reference for both the RP and cytotoxicity tests. Data were statistically analyzed using One-Way ANOVA and Tukey's test (p≤0.05). RESULTS: All adhesives exhibited similar DC (p=0.1931). The RP of adhesives was improved with the addition of up to 5wt.% of HNTs (p<0.001). Adhesives containing 5-10wt.% of HNTs led to greater KHN when compared to the control (p<0.001). The FS was reduced only when 20wt.% of HNTs was added (p≤0.001). None of the prepared adhesives was cytotoxic. CONCLUSION: The incorporation of up to 10wt.% of HNTs into the adhesive resins did not jeopardize the tested physical and biological properties. CLINICAL SIGNIFICANCE: When using HNTs as carriers of drugs/bioactive compounds, the amount of the former added into adhesive resin materials should not exceed 10wt.%; otherwise, a significant reduction in physicomechanical properties may be expected.

Effect of the addition of silanated silica on the mechanical properties of microwave heat-cured acrylic resin.

OBJECTIVES: The purpose of this study was to evaluate the flexural strength and Vickers hardness of a microwave energy heat-cured acrylic resin by adding different concentrations of silane surface-treated nanoparticle silica. METHODS: Acrylic resin specimens with dimensions of 65 × 10 × 2.5 mm were formed and divided into five experimental groups (n = 10) according to the silica concentration added to the acrylic resin mass (weight %) prior to polymerisation : G1, without silica; G2, 0.1% silica; G3, 0.5% silica; G4, 1.0% silica; and G5, 5.0% silica. The specimens were submitted to a three-point flexural strength test and to the Vickers hardness test (HVN). The data obtained were statistically analysed by anova and the Tukey test (α = 0.05). RESULTS: Regarding flexural strength, G5 differed from the other experimental groups (G1, G2, G3 and G4) presenting the lowest mean, while G4 presented a significantly higher mean, with the exception of group G3. Regarding Vickers hardness, a decrease in values was observed, in which G1 presented the highest hardness compared with the other experimental groups. CONCLUSION: Incorporating surface-treated silica resulted in direct benefits in the flexural strength of the acrylic resin activated by microwave energy; however, similar results were not achieved for hardness.