Mechanical-physicochemical properties and biocompatibility of catechin-incorporated adhesive resins

Abstract Several anti-proteolytic dentin therapies are being exhaustively studied in an attempt to reduce dentin bond degradation and improve clinical performance and longevity of adhesive restorations. Objectives This study assessed the effect of epigallocatechin-3-gallate (EGCG) on long-term bond strength when incorporated into adhesives. Material and Methods Adhesive systems were formulated with EGCG concentrations of 0 wt%: (no EGCG; control); 0.5 wt% EGCG; 1.0 wt% EGCG, and 1.5 wt% EGCG. Flexural strength (FS), modulus of elasticity (ME), modulus of resilience (MR), compressive strength (CS), degree of conversion (DC), polymerization shrinkage (PS), percentage of water sorption (%WS), percentage of water solubility (%WL) and cytotoxicity properties were tested. Dentin microtensile bond strength (µTBS) was evaluated after 24 h and again after 6 months of water storage. The adhesive interface was analyzed using scanning electron microscopy (SEM). Results No significant differences were found among the groups in terms of FS, ME, MR, CS and PS. EGCG-doped adhesives increased the DC relative to the control group. EGCG concentrations of 1.0 wt% and 0.5 wt% decreased the WS of adhesives. WL decreased in all cases in which EGCG was added to adhesives, regardless of the concentration. EGCG concentrations of 1.0 wt% and 0.5 wt% reduced cytotoxicity. EGCG concentrations of 1.0 wt% and 0.5 wt% preserved µTBS after 6 months of storage, while 1.5 wt% EGCG significantly decreased µTBS. SEM: the integrity of the hybrid layer was maintained in the 0.5 wt% and 1.0 wt% EGCG groups. Conclusion EGCG concentrations of 1.0 wt% and 0.5 wt% showed better biological and mechanical performance, preserved bond strength and adhesive interface, and reduced cytotoxicity.

Long-term bonding efficacy of adhesives containing benzodioxioles as alternative co-initiators

Abstract This study evaluated the three-year lifespan of the bond to dentin of experimental self-etch adhesives containing benzodioxole derivatives - 1,3-benzodioxole (BDO) and piperonyl alcohol (PA) - as co-initiator alternative to amines. Adhesive resins were formulated using Bis-GMA, TEGDMA, HEMA, camphorquinone and different co-initiators: BDO, PA or ethyl 4-dimethylamino benzoate (EDAB - amine). An experimental self-etch primer was used to complete the two-step, self-etch adhesive system. Clearfil SE Bond (CSE) was used as commercial reference. Bond strength to human dentin was assessed by microtensile bond strength (µTBS) test, and failure mode was classified. Morphology of the dentin bonding interface was assessed via scanning electron microscopy (SEM). Irrespective of the dental adhesives evaluated, µTBS was higher after 24 hours compared with that after 1.5 and 3 years (p ≤ 0.001). However, adhesives with BDO and PA as co-initiators showed significantly higher bond strength than the bonding resin with EDAB (p ≤ 0.002), independent of the time evaluated. The commercial adhesive CSE showed similar bond strength compared with the other groups (p ≥ 0.05). Mixed failures were mainly observed after 24 hours, while adhesive failures were more frequently observed after 1.5 and 3 years. No notable differences in homogeneity and continuity along the bonded interfaces were detected among the materials in the SEM analysis. In conclusion, benzodioxole derivatives are feasible alternative co-initiators to tertiary amine in camphorquinone-based self-etching dental adhesive formulations.

Influence of a hydrophobic monomer on the physical and mechanical properties of experimental surface sealants

Abstract This study evaluated the effect of adding the hydrophobic monomer 1,12 dodecanediol dimethacrylate (DDDMA) to experimental sealants with and without thermocycling on degree of conversion (DC), water sorption (WS), water solubility (WSB), color stability (ΔE), and micro-shear bond strength (μSBS). Five experimental and one commercially available sealant (Bisco - BIS) were tested. The experimental sealants were formulated by mixing different percentages of DDDMA monomers and urethane dimethacrylate (UDMA). The photoinitiator system was composed by camphorquinone (CQ) and tertiary amine 4-ethyl benzoate dimetilamiono (EDBA). Ethanol was used as a solvent. The experimental groups were named sequentially according to the monomeric content (DDDMA/UDMA): S40/40 (40/40), S50/30 (50/30), S60/20 (60/20), S70/10 (70/10) and S80/0 (80/0). Data were analyzed separately by one-way ANOVA, followed by Tukey's test (p<0.05). The values of DC ranged from 94.59% (S40/40) to 54.02% (S80/10). BIS showed the highest WS value (p<0.05) and S40/40, S50/30, S60/20 and S80/0 showed the lowest WS values of all tested sealants. WSB values ranged from 7.88 µg/mm3 (BIS) to 13.27 µg/mm3 (S70/10). The highest ΔE value was 11.05±2.88 for BIS and the highest μSBS value was found for S60/20. No significant difference was observed in bond strength between sealants and bovine enamel after thermocycling. Adding DDDMA to the composition of surface sealants can improve its performance, once the monomer increased the degree of conversion and the color stability.

Influence of Different Concentration and Ratio of a Photoinitiator System on the Properties of Experimental Resin Composites

Abstract The aim in this study was to evaluate the influence of different ratio of camphorquinone/tertiary amine concentration on the flexural strength (FS), elastic modulus (EM), degree of conversion (DC), yellowing (YL), water sorption (WS) and water solubility (WSL) of experimental composites. Thus, acrylate blends were prepared with different camphorquinone (CQ) and amine (DABE) concentrations and ratios by weight: (CQ/DABE%): 0.4/0.4% (C1), 0.4/0.8% (C2), 0.6/0.6% (C3), 0.6/1.2% (C4), 0.8/0.8% (C5), 0.8/1.6% (C6), 1.0/1.0% (C7), 1.0/2.0% (C8), 1.5/1.5% (C9), 1.5/3.0% (C10). For the FS and EM, rectangular specimens (7x2x1 mm, n=10) were photo-activated by single-peak LED for 20 s and tested at Instron (0.5 mm/min). Then, the same specimens were evaluated by FTIR for DC measurement. For YL, disks (5x2 mm, n=10) were prepared, light-cured for 20 s and evaluated in spectrophotometer using the b aspect of the CIEL*a*b* system. For WS and WSL, the volume of the samples was calculated (mm³). For WS and WSL, composites disks (5x0.5 mm, n=5) were prepared. After desiccation, the specimens were stored in distilled water for 7 days and again desiccated, in order to measure the WS and WSL. Data were submitted to one-way ANOVA and Tukey's test (5%). The groups C8, C9 and C10 showed higher DC, EM and YL means, compared to other composites. Therefore, the FS and WS values were similar among all groups. Also, C1, C2 and C3 presented higher WSL in 7 days, compared to other composites. In general, higher concentrations of camphorquinone promoted higher physical-mechanical properties; however, inducing higher yellowing effect for the experimental composites

Resumo O objetivo foi avaliar a influência da concentração e proporção de canforoquinona (CQ)/amina terciária (DABE) na resistência à flexão (RF), módulo flexural (MF), grau de conversão (GC), amarelamento (AM), sorpção (SA) e solubilidade em água (SL) de compósitos experimentais. Blendas acrilatas foram preparadas com diferentes concentrações e proporções de CQ/DABE em peso, como segue: (CQ/DABE%): 0,4/0,4% (C1); 0,4/0,8% (C2); 0,6/0,6% (C3); 0,6/1,2% (C4); 0,8/0,8% (C5); 0,8/1,6% (C6); 1,0/1,0% (C7); 1,0/2,0% (C8); 1,5/1,5% (C9); 1,5/3,0% (C10). Para RF e MF, espécimes retangulares (7x2x1 mm, n=10) foram fotoativados com LED de pico único (Radii Cal) por 20 s e testados em máquina Instron (0,5 mm/min). Após, o GC dos mesmos espécimes (fragmentos) foi mensurado por FTIR. Para AM, discos de compósito (5x2 mm, n=10) foram preparados, fotoativados por 20 s e imediatamente avaliados em espectrofotômetro, considerando o aspecto b do sistema CIEL*a*b*. Para SA e SL, discos de compósito (5x0,5 mm, n=5) foram preparados e seus volumes calculados (mm³). Após desidratação, as amostras foram pesadas e armazenadas em água destilada por 7 dias, pesadas e novamente desidratadas e pesadas, para se calcular o SA e SL. Os dados foram submetidos a one-way ANOVA e teste de Tukey (5%). Os grupos C8, C9 e C10 mostraram maior GC, MF e AM, comparado aos outros grupos. No entanto, RF e SA foram similares entre todos os grupos. Ainda, C1, C2 e C3 apresentaram maior SL em 7 dias comparado aos outros grupos. Em geral, maiores concentrações de CQ promoveram melhores propriedades físico-mecânicas; no entanto, levaram ao maior amarelamento dos compósitos.

Mechanical properties, water sorption characteristics, and compound release of grape seed extract-incorporated resins

Abstract Objective This study evaluated the effect of grape seed extract (GSE) incorporation on the mechanical properties, water sorption, solubility, and GSE release from the experimental adhesive resins. Material and Methods An experimental comonomer mixture, consisting of 40% Bis-GMA, 30% Bis MP, 28% HEMA, 0.26% camphorquinone and 1% EDMAB, was used to prepare four GSE-incorporated adhesive resins at concentrations of 0.5, 1, 1.5, and 2 wt%. The neat resin without GSE was used as the control. Six resin beams (25 mm x 2 mm x 2 mm) per group were prepared for flexural strength and modulus of elasticity evaluations using a universal testing machine at a crosshead speed of 1 mm/min. Five disks (6 mm in diameter and 2 mm in thickness) per group were used for microhardness measurements using a Leitz micro-hardness tester with Leica Qgo software. Five disks (7 mm in diameter and 2 mm in thickness) per group were prepared and stored in deionized water for 28 days. Water sorption, solubility, and GSE release in deionized water were calculated for each GSE-incorporated adhesive at the end of 28th day. Data was evaluated using one-way ANOVA and Tukey multiple comparisons. Results Flexural strength, modulus of elasticity and microhardness of GSE-incorporated adhesive decreased significantly with incorporation of 1.5% of GSE (p<0.05). Addition of GSE had no effect on the water sorption of the adhesive resins (p=0.33). The solubility of the resin also increased significantly with incorporation of 1.5% of GSE (p<0.05). Quantities of GSE release increased with increased concentration of GSE in the adhesive resin. Conclusion Up to 1% of GSE can be incorporated into a dental adhesive resin without interfering with the mechanical properties or solubility of the resins.

Evaluation of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental dental resin-based materials

ABSTRACT Objective To evaluate the influence of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental resin-based materials photoactivated using different light curing units (LCUs). Material and Methods Experimental resin-based materials with the same organic matrix (60:40 wt% BisGMA:TEGDMA) were mechanically blended using a centrifugal mixing device. To this blend, different photoinitiator systems were added in equimolar concentrations with aliphatic amine doubled by wt%: 0.4 wt% CQ; 0.38 wt% PPD; or 0.2 wt% CQ and 0.19 wt% PPD. The degree of conversion (DC), flexural strength (FS), Young’s modulus (YM), Knoop hardness (KNH), crosslinking density (CLD), and yellowing (Y) were evaluated (n=10). All samples were light cured with the following LCUs: a halogen lamp (XL 2500), a monowave LED (Radii), or a polywave LED (Valo) with 16 J/cm2. The results were analysed by two-way ANOVA and Tukey’s test (α=0.05). Results No statistical differences were found between the different photoinitiator systems to KNH, CLS, FS, and YM properties (p≥0.05). PPD/CQ association showed the higher DC values compared with CQ and PPD isolated systems when photoactivated by a polywave LED (p≤0.05). Y values were highest for the CQ compared with the PPD systems (p≤0.05). Conclusion PPD isolated system promoted similar chemical and mechanical properties and less yellowing compared with the CQ isolated system, regardless of the LCU used.

Photoelastic evaluation of the effect of composite formulation on polymerization shrinkage stress

We compared polymerization stress in two commercial composites and three experimental composites made using camphorquinone (CQ) and/or phenylpropanedione (PPD) as photoinitiators. The internal surfaces of photoelastic resin discs with cylindrical cavities were roughened and treated with adhesive. Composites were divided into five groups: two commercial composites (Filtek Silorane and Filtek Z250) and three experimental composites with CQ/amine, CQ/PPD/amine, and PPD/amine. Composites were photopolymerized inside cavities, and subjected to photoelastic analysis immediately and at 24 hours and 7 days later using a plane polariscope. Stress created by Silorane (3.08 ± 0.09 MPa) was similar to that of Z250 (3.19 ± 0.13 MPa) immediately after photopolymerization (p > 0.05). After 24 hours and 7 days, Z250 (3.53 ± 0.15 and 3.69 ± 0.10 MPa, respectively) showed higher stress than Silorane (3.19 ± 0.10 and 3.16 ± 0.10 MPa, respectively). Qualitative analysis immediately after photopolymerization showed composite/CQ promoted higher stress than PPD, but stress levels at other evaluated times were statistically similar, varying between 3.45 ± 0.11 MPa and 3.92 ± 0.13 MPa. At 24 hours and 7 days, Silorane created the lowest stress. All photoinitiators created comparable tensions during polymerization.

Influence of different light sources on the conversion of composite resins.

Aims: The purpose of this paper was to evaluate the influence of different light curing units on the conversion of four composite resins with different compositions (Durafill VS® - Heraeus-Kulzer, Tetric Ceram® - Ivoclar/Vivadent, Filtek™ Supreme XT - 3M ESPE™ e Aelite™ LS Packable - Bisco), using differential scanning calorimetry. Materials and Methods: A stainless steel matrix was used to prepare 48 cylindrical composite test samples (n=6), measuring 3 mm in diameter and 1 mm in thickness. The samples were photoactivated using a halogen lamp (Optilux™ 500 - Demetron/Kerr) and three different generations of light-emitting diodes (LEDs) (LEC-470 I - MMOptics, Radii Plus - SDI and Ultra-Lume™ LED 5 - Ultradent). After removal of the matrix, each sample was weighed and hermetically sealed in an aluminum pan and analyzed. The amount of heat liberated by thermopolymerisation of residual monomers after photoactivation was measured in Joules/gram (J/g). The data were submitted to Analysis of Variance (ANOVA) test (P ≤ 0.002) and the Tukey test (P < 0.05). Results: The Ultra-Lume™ LED 5 was superior on degree of conversion for all resins. The Radii Plus was equal to the Ultra-Lume™ LED 5, except for the resin Tetric Ceram® , were the Optilux™ 500 was superior. The LEC-470 I was inferior for the conversion of all resins. Conclusion: The study proves the importance of the compatibility of the different photoinitiators in resin composites with the different light sources.

Effect of different photo-initiators and light curing units on degree of conversion of composites

The aim of this study was to evaluate: (i) the absorption of photo-initiators and emission spectra of light curing units (LCUs); and (ii) the degree of conversion (DC) of experimental composites formulated with different photo-initiators when activated by different LCUs. Blends of BisGMA, UDMA, BisEMA and TEGDMA with camphorquinone (CQ) and/ or 1-phenyl-1,2-propanedione (PPD) were prepared. Dimethylaminoethyl methacrylate (DMAEMA) was used as co-initiator. Each mixture was loaded with 65 wt percent of silanated filler particles. One quartz-tungsten-halogen - QTH (XL 2500, 3M/ESPE) and two lightemitting diode (LED) LCUs (UltraBlue IS, DMC and UltraLume LED 5, Ultradent) were used for activation procedures. Irradiance (mW/cm²) was calculated by the ratio of the output power by the area of the tip, and spectral distribution with a spectrometer (USB 2000). The absorption curve of each photo-initiator was determined using a spectrophotometer (Varian Cary 5G). DC was assessed by Fourier transformed infrared spectroscopy. Data were submitted to two-way ANOVA and Tukey's test (5 percent). No significant difference was found for DC values when using LED LCUs regardless of the photo-initiator type. However, PPD showed significantly lower DC values than composites with CQ when irradiated with QTH. PPD produced DC values similar to those of CQ, but it was dependent on the LCU type.