The effect of photoinitiator type and filler load on physicochemical and mechanical properties of experimental light-cured resin cements through lithium disilicate ceramics of different shades and thicknesses.

OBJECTIVE: This study investigated the influence of photoinitiator types on degree of conversion (DC), rate of polymerization (RP), flexural strength (FS), flexural modulus (FM), and light transmittance (LT) of filled and unfilled light-curable resin cements through different thicknesses and shades of lithium disilicate ceramics. METHODS: Lithium disilicate ceramic discs (IPS Emax Press, background [0.0], 0.5, 1.0, 2.0, 3.0, and 4.0 mm, shades A1 and BL3) were prepared. Experimental resin-based cements [TEGDMA/BisGMA (50/50 mass%)] were prepared using either camphorquinone (CQ)/amine (0.44/1.85 mol%) or TPO (0.44 mol%)], and a micro and nanofiller loads of nil (unfilled); 40/10 mass%; and 50/10 mass%). Resin cements (0.2 mm thick) were placed on the lower surface of the ceramic specimens and light-activated for 30 s from the upper surface using a Bluephase Style curing light (exitance at tip: 1236 mW/cm2 ± 1.20). LT and distribution of irradiance through the ceramics were measured using a UV-vis spectrometer and a beam profile camera, respectively (n = 3). The DC and RP were measured in real-time using mid infrared spectroscopy in attenuated total reflectance (ATR) mode (n = 3). FS and FM were measured using a universal testing machine (n = 5). Statistical analyses were performed on LT, DC, RP, FS, and FM data using a general linear model, and supplementary ANOVA and post hoc Tukey multiple comparison test were also performed (α = .05). RESULTS: Thicknesses, shades, photoinitiator type, and fillers load significantly influenced the optical and mechanical characteristics of the resin-based materials (p < 0.05). The BL3 shade ceramic provided higher values of DC, RP, FS, FM, and LT compared with the A1 shade (p < 0.05). Increasing ceramic thickness decreased the properties of the resin-based materials (p < 0.05). Generally, TPO improved mechanical properties of the resin cement compared with CQ (p < 0.05). SIGNIFICANCE: The luting process of indirect restorations may be improved by using high molar absorptivity, more reactive, and more efficient photoinitiators such as TPO, as opposed to conventional CQ. The use of such initiator may allow the placement of thicker and more opaque indirect restorations.

Degree of Conversion and Mechanical Properties of a Commercial Composite with an Advanced Polymerization System.

Advanced Polymerization System (APS) technology in a commercial composite resin enables reduction of the concentration of camphorquinone without altering composite physicochemical properties. AIM: The aim of this study was to evaluate the degree of conversion and mechanical properties of a commercial composite with an advanced polymerization system (APS) and compare it to other composites that do not use this system. MATERIALS AND METHOD: Five groups were analyzed. Group 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). Degree of conversion (DC, n=3) was analyzed immediately and after 24h by analysis with FTIR spectroscopy. For Knoop hardness (KHN, n=3), 5 indentations were made at the top and bottom of specimens 2 mm thick. Flexural strength (FS, n=10) was determined by the three-point method in a universal testing machine. Polymerization stress (PS) was determined by light-curing the material (1.0 mm high) between polymethylmethacrylate rods in a universal testing machine. Light curing was performed with a Valo Cordless LED (1,000 mW/cm2 x 20 s: 20J). The results were analyzed using ANOVA and complemented by Tukey's test (α=0.05). RESULTS: The highest DC values (immediate and 24h after) were observed for VT and OP resins, followed by FZ, AU and ES. FZ (top and bottom) had the highest KHN values, similar to VT top. AU, ES, OP and VT had statistically different KHN between their top and bottom surfaces. The highest RF values were observed for FZ, followed by OP/VT, ES and AU. The highest TP values were observed for FZ, OP and VT. CONCLUSION: The Vittra APS resin with a new polymerization system presents satisfactory performance for the parameters evaluated.

A tecnologia Advanced Polymerization System (APS) presente em uma resina composta comercial permite reduzir a concentração de canforoquinona sem alterar as propriedades físico-químicas do compósito. Objetivo: o objetivo deste estudo foi avaliar o grau de conversão e as propriedades mecânicas de um compósito comercial com sistema avançado de polimerização (SAP) e comparálo com outros compósitos que não utilizam esse sistema. Materiais e Método: cinco grupos foram analisados. Grupo 1 (VT: Vittra APS - FGM); G2 (AU: Aura ­ SDI); G3 (ES: Quick Sigma Stelite ­ TOKOYAMA); G4 (FZ: Filtek Z350 XT ­ 3M ESPE); G5 (OP: Opallis -FGM). O grau de conversão (GC, n=3) foi analisado imediatamente e após 24h através da análise com espectroscopia FTIR; para dureza Knoop (DK, n=3), foram feitas 5 indentações no topo e na base de corpos de prova de 2 mm de espessura; para determinar a resistência à flexão (RF, n=10), o método de três pontos foi realizado em uma máquina universal de ensaios; a tensão de polimerização (TP) foi determinada pela fotopolimerização do material (1,0 mm de altura) entre hastes de polimetilmetacrilato em uma máquina de teste universal. A fotopolimerização foi realizada com um Valo Cordless LED (1.000 mW/cm2 x 20 s: 20J). Os resultados foram analisados por ANOVA e complementados pelo teste de Tukey (α=0,05). Resultados: os maiores valores de GC (imediato e 24h após) foram observados para as resinas VT e OP, seguidas de FZ, AU e ES. A resina FZ (superior e inferior) apresentou os maiores valores de DK, semelhante ao VT superior. As resinas AU, ES, OP e VT apresentaram DK estatisticamente diferente entre suas superfícies de topo e base. Os maiores valores de RF foram observados para FZ, seguido de OP/VT, ES e AU. Os maiores valores de TP foram observados para FZ, OP e VT. Conclusão: com base nos resultados, pode-se concluir que a resina Vittra APS com um novo sistema de polimerização apresenta desempenho satisfatório para os parâmetros avaliados.

Degree of Conversion and Mechanical Properties of a Commercial Composite with an Advanced Polymerization System / Avaliação do grau de conversão e das propriedades mecânicas de um compósito comercial com sistema avançado de polimerização

ABSTRACT Advanced Polymerization System (APS) technology in a commercial composite resin enables reduction of the concentration of camphorquinone without altering composite physicochemical properties. Aim: The aim of this study was to evaluate the degree of conversion and mechanical properties of a commercial composite with an advanced polymerization system (APS) and compare it to other composites that do not use this system. Materials and Method: Five groups were analyzed. Group 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). Degree of conversion (DC, n=3) was analyzed immediately and after 24h by analysis with FTIR spectroscopy. For Knoop hardness (KHN, n=3), 5 indentations were made at the top and bottom of specimens 2 mm thick. Flexural strength (FS, n=10) was determined by the three-point method in a universal testing machine. Polymerization stress (PS) was determined by light-curing the material (1.0 mm high) between polymethylmethacrylate rods in a universal testing machine. Light curing was performed with a Valo Cordless LED (1,000 mW/cm2 x 20 s: 20J). The results were analyzed using ANOVA and complemented by Tukey's test (α=0.05). Results: The highest DC values (immediate and 24h after) were observed for VT and OP resins, followed by FZ, AU and ES. FZ (top and bottom) had the highest KHN values, similar to VT top. AU, ES, OP and VT had statistically different KHN between their top and bottom surfaces. The highest RF values were observed for FZ, followed by OP/VT, ES and AU. The highest TP values were observed for FZ, OP and VT. Conclusion: The Vittra APS resin with a new polymerization system presents satisfactory performance for the parameters evaluated.

RESUMO A tecnologia Advanced Polymerization System (APS) presente em uma resina composta comercial permite reduzir a concentração de canforoquinona sem alterar as propriedades físico-químicas do compósito. Objetivo: o objetivo deste estudo foi avaliar o grau de conversão e as propriedades mecânicas de um compósito comercial com sistema avançado de polimerização (SAP) e comparálo com outros compósitos que não utilizam esse sistema. Materiais e Método: cinco grupos foram analisados. Grupo 1 (VT: Vittra APS - FGM); G2 (AU: Aura - SDI); G3 (ES: Quick Sigma Stelite - TOKOYAMA); G4 (FZ: Filtek Z350 XT - 3M ESPE); G5 (OP: Opallis -FGM). O grau de conversão (GC, n=3) foi analisado imediatamente e após 24h através da análise com espectroscopia FTIR; para dureza Knoop (DK, n=3), foram feitas 5 indentações no topo e na base de corpos de prova de 2 mm de espessura; para determinar a resistência à flexão (RF, n=10), o método de três pontos foi realizado em uma máquina universal de ensaios; a tensão de polimerização (TP) foi determinada pela fotopolimerização do material (1,0 mm de altura) entre hastes de polimetilmetacrilato em uma máquina de teste universal. A fotopolimerização foi realizada com um Valo Cordless LED (1.000 mW/cm2 x 20 s: 20J). Os resultados foram analisados por ANOVA e complementados pelo teste de Tukey (α=0,05). Resultados: os maiores valores de GC (imediato e 24h após) foram observados para as resinas VT e OP, seguidas de FZ, AU e ES. A resina FZ (superior e inferior) apresentou os maiores valores de DK, semelhante ao VT superior. As resinas AU, ES, OP e VT apresentaram DK estatisticamente diferente entre suas superfícies de topo e base. Os maiores valores de RF foram observados para FZ, seguido de OP/VT, ES e AU. Os maiores valores de TP foram observados para FZ, OP e VT. Conclusão: com base nos resultados, pode-se concluir que a resina Vittra APS com um novo sistema de polimerização apresenta desempenho satisfatório para os parâmetros avaliados.

Pore Structure Tuning of Poly-EGDMA Biomedical Material by Varying the O-Quinone Photoinitiator.

Porous polymer monoliths with thicknesses of 2 and 4 mm were obtained via polymerization of ethylene glycol dimethacrylate (EGDMA) under the influence visible-light irradiation in the presence of a 70 wt% 1-butanol porogenic agent and o-quinone photoinitiators. The o-quinones used were: 3,5-di-tret-butyl-benzoquinone-1,2 (35Q), 3,6-di-tret-butyl-benzoquinone-1,2 (36Q), camphorquinone (CQ), and 9,10-phenanthrenequinone (PQ). Porous monoliths were also synthesized from the same mixture but using 2,2'-azo-bis(iso-butyronitrile) (AIBN) at 100 °C instead o-quinones. According to the results of scanning electron microscopy, all the resulting samples were conglomerates of spherical, polymeric particles with pores between them. Use of mercury porometry showed that the interconnected pore systems of all the polymers were open. The average pore size, Dmod, in such polymers strongly depended on both the nature of the initiator and the method of initiation of polymerization. For polymers obtained in the presence of AIBN, the Dmod value was as low as 0.8 µm. For polymers obtained via photoinitiation in the presence of 36Q, 35Q, CQ, and PQ, the Dmod values were significantly greater, i.e., 9.9, 6.4, 3.6, and 3.7 µm, respectively. The compressive strength and Young's modulus of the porous monoliths increased symbatically in the series PQ < CQ < 36Q < 35Q < AIBN with decreasing proportions of large pores (over 12 µm) in their polymer structures. The photopolymerization rate of the EGDMA and 1-butanol, 30:70 wt% mixture was maximal for PQ and minimal for 35Q. All polymers tested were non-cytotoxic. Based on the data from MTT testing, it can be noted that the polymers obtained via photoinitiation were characterized by their positive effect on the proliferative activity of human dermal fibroblasts. This makes them promising osteoplastic materials for clinical trials.

Extension of the working time of dental composites due to a new type of white operating lamp.

OBJECTIVES: Dental composite materials for filling teeth are usually hardened by polymerisation lamps emitting blue light. However, the same wavelength is also emitted by light of dental operating lamps for lighting the oral cavity. Thus, the hardening of the composite is already initiated earlier, shortening the time of formability. The objective of this study is to develop a specific white LED for dental operating lamps. When restoring teeth, it enables dentists to work longer on light-curing composites in the same brightness. METHODS: Based on a short-wave blue coloured LED and a fluorescent substance, a white luminescent LED with a colour temperature of approx. 3,000 K is produced as a prototype. The formable working times of three composites are measured for this LED and two dental head lamps at an illuminance of 10,000 lx. RESULTS: Shorter working times of 98-237 s were measured for the headlamps and 409-807 s for the new LED. This light of the new LED is perceived by the human eye as warm white. CONCLUSIONS: The new LED extends the working time by the factor of 3.0 to 5.8 compared to the head lamps. This enables more precise modelling of fillings.

Evaluation of the Selected Mechanical and Aesthetic Properties of Experimental Resin Dental Composites Containing 1-phenyl-1,2 Propanedione or Phenylbis(2,4,6-trimethylbenzoyl)-phosphine Oxide as a Photoinitiator.

The goal of this study was to compare the mechanical properties of experimental resin dental composites containing a conventional photoinitiating system (camphorquinone CQ and 2-(dimethylami-no)ethyl methacrylate (DMAEMA)) to a photoinitiator system containing 1-phenyl-1,2 propanedione (PPD) with 2-(dimethylami-no)ethyl methacrylate) or acting alone phenylbis(2,4,6-trimethylbenzoyl)-phosphine oxide (BAPO). The manually produced composites consisted of an organic matrix: bis-GMA (60 wt. %), TEGDMA (40 wt. %), and silanized silica filler (45 wt. %). The composites contained 0.4/0.8 wt. %, 0.8/1.6 wt. %, and 1/2 wt. % of PPD/DMAEMA and another group included 0.25, 0.5, or 1 wt. % of BAPO. Vickers hardness, microhardness (in the nanoindentation test), diametral tensile strength, and flexural strength were assessed, and CIE L* a* b* colorimetric analysis was conducted for each composite produced. The highest average Vickers hardness values were obtained for the composite containing 1 wt. % BAPO (43.73 ± 3.52 HV). There was no statistical difference in the results of diametral tensile strength for the experimental composites tested. The results of 3-point bending tests were the highest for composites containing CQ (77.3 ± 8.84 MPa). Despite the higher hardness of experimental composites including PPD or BAPO, compared with composites with CQ, the overall results indicate that the composite with CQ still represents a better solution when used as a photoinitiator system. Moreover, the composites containing PPD and DMAEMA are not promising in terms of color or mechanical properties, especially as they require significantly longer irradiation times.

Lignin-derived new hydrogen donors for photoinitiating systems in dental materials.

OBJECTIVES: The aim of this study is to develop amine free photo-initiating system (PIs) for the photopolymerization of dental methacrylate resins, using seven new hydrogen donors HDA-HDG derived from ß-O-4 lignin model. METHODS: Seven experimental CQ/HD PIs were formulated with Bis-GMA/TEGDMA (70 w%/30 w%). CQ/EDB system was chosen as the comparison group. FTIR-ATR was used to monitor the polymerization kinetics and double bond conversion. Bleaching property and color stability were evaluated using a spectrophotometer. Molecular orbitals calculations were used to demonstrate C-H bond dissociation energies of the novel HDs. Depth of cure of the HD based systems were compared to the EDB based one. Cytotoxicity was also studied by CCK8 assay using tissue of mouse fibroblasts (L929 cells). RESULTS: Compared to CQ/EDB system, the new CQ/HD systems show comparable or better photopolymerization performances (1 mm-thick samples). Comparable or even better bleaching properties were also obtained with the new amine-free systems. Comparing to EDB, all HDs exhibited significantly lower C-H bond dissociation energies by molecular orbitals calculations. Groups with new HD showed higher depth of cure. OD and RGR values were similar to that of the CQ/EDB group, ensuring the feasibility of the new HDs in dental materials. CLINICAL SIGNIFICANCE: The new CQ/HD PI systems could be potentially useful in dental materials, presenting improvements in restorations' esthetic and biocompatibility.

Melatonin Mitigates iNOS-Related Effects of HEMA and Camphorquinone in Human Dental Pulp Cells: Relevance for Postoperative Sensitivity Mechanism in Type 2 Diabetes.

High elution and diffusion of 2-hydroxylethyl methacrylate (HEMA) and camphorquinone (CQ) through dentinal tubules may induce pulp injury and postoperative sensitivity. We aimed to investigate the melatonin protective effect in HEMA- and CQ-treated human dental pulp cells (hDPCs) as well as its relevance in a mechanism for postoperative sensitivity in diabetic patients. hDPCs were exposed to HEMA (5 mM) and/or CQ (1 mM) in the absence and presence of melatonin (MEL) (0.1 mM and 1 mM). Heme oxygenase-1 (HMOX1), NADPH oxidase-4 (NOX4), BCL-2-associated X-protein (BAX), B-cell lymphoma-2 (BCL-2) and caspase-3 (CASP3) gene expression levels, and superoxide dismutase (SOD) activity were measured in hDPCs while inducible nitric oxide synthase (iNOS) and melatonin protein expression were measured in human dental pulp as well, by RT-PCR, by ELISA, and spectrophotometrically. Bioinformatic analyses were performed by using the ShinyGO (v.0.75) application. Type 2 diabetic patients showed a higher incidence of postoperative sensitivity and lower melatonin and higher iNOS content in dental pulp tissue compared with non-diabetic patients. Melatonin, when co-added in hDPC culture, reverses HEMA and CQ cytotoxic effects via anti-apoptotic and anti-inflammatory/antioxidant iNOS-related effects. Enrichment analyses showed that genes/proteins, altered by HEMA and CQ and normalized by melatonin, are the most prominently overrepresented in type 2 diabetes mellitus pathways and that they share subcellular localization in different oligomeric protein complexes consisting of anti- and pro-apoptotic regulators. This is the first evidence of the ability of melatonin to counteract iNOS-mediated inflammatory and stress effects in HEMA- and CQ-treated hDPCs, which could be of significance for the modulation of presently observed immediate postoperative sensitivity after composite restoration in type 2 diabetic patients.

Inducing cathepsin L expression/production, lysosomal activation, and autophagy of human dental pulp cells by dentin bonding agents, camphorquinone and BisGMA and the related mechanisms.

Camphorquinone (CQ) and resin monomers are included in dentin bonding agents (DBAs) and composite resin to restore tooth defects due to abrasion, crown fracture, or dental caries. DBAs, CQ, and bisphenol A-glycidyl methacrylate (BisGMA) applications influence the biological activities of the dental pulp. The current investigation aimed to delineate the effect of DBAs, CQ, and BisGMA on cathepsin L production/expression, lysosomal activity, and autophagy induction in human dental pulp cells (HDPCs). HDPCs were exposed to DBAs, CQ, or BisGMA with/without inhibitors for 24 h. Enzyme-linked immunosorbent assay was employed to determine the cathepsin L level in culture medium. The cell layer was utilized to measure cell viability by 3-(4,5-dimethyl-thiazol-2-yl)-2,5-diphenyl -tetrazolium bromide (MTT) assay. Real-time PCR was used to evaluate the mRNA expression. Western blotting or immunofluorescent staining was used to study protein expression. Lysosomal density was evaluated by lysotracker red staining. We found that DBAs, CQ, and BisGMA stimulated cathepsin L mRNA, protein expression, and production in HDPCs. In addition, CQ and BisGMA induced lysosomal activity, Beclin1, ATG12, LC3B, Bax, and p53 expression in HDPCs, indicating the stimulation of autophagy. Glutathione (GSH) prevented CQ- and BisGMA-induced cytotoxicity. Moreover, E64d, cathepsin L inhibitor (two cathepsin inhibitors), and Pifithrin-α (a p53 inhibitor) showed little preventive effect toward CQ- and BisGMA-induced cytotoxicity. Autophagy inhibitors (NH4Cl, Lys05) mildly enhanced the CQ- and BisGMA-induced cytotoxicity. These results indicate that DBAs stimulated cathepsin L, possibly due to their content of CQ and BisGMA that may induce cathepsin L in HDPCs. CQ and BisGMA stimulated lysosomal activity, autophagy, and apoptosis, possibly via induction of Beclin 1, ATG12, LC-3B, Bax, and p53 expression. In addition, CQ and BisGMA cytotoxicity was related to redox change and autophagy. These events are important role in pulpal changes after the restoration of tooth decay using CQ- and BisGMA-containing DBAs and resin composite.

Can TPO as Photoinitiator Replace "Golden Mean" Camphorquinone and Tertiary Amines in Dental Composites? Testing Experimental Composites Containing Different Concentration of Diphenyl(2,4,6-trimethylbenzoyl)phosphine Oxide.

The aim of this research was to compare the biomechanical properties of experimental composites containing a classic photoinitiating system (camphorquinone and 2-(dimethylami-no)ethyl methacrylate) or diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO) as a photoinitiator. The produced light-cured composites consisted of an organic matrix-Bis-GMA (60 wt.%), TEGDMA (40 wt.%) and silanized silica filler (45 wt.%). Composites contained 0.27; 0.5; 0.75 or 1 wt.% TPO. Vickers hardness, microhardness (in the nanoindentation test), diametral tensile strength, resistance to three-point bending and the CIE L* a* b* colorimetric analysis was performed with each composite produced. The highest average Vickers hardness values were obtained for the composite containing 1 wt.% TPO (43.18 ± 1.7HV). The diametral tensile strength remains on regardless of the type and amount of photoinitiator statistically the same level, except for the composite containing 0.5 wt.% TPO for which DTS = 22.70 ± 4.7 MPa and is the lowest recorded value. The highest average diametral tensile strength was obtained for the composite containing 0.75 wt.% TPO (29.73 ± 4.8 MPa). The highest modulus of elasticity characterized the composite containing 0.75 wt.% TPO (5383.33 ± 1067.1 MPa). Composite containing 0.75 wt.% TPO has optimal results in terms of Vickers hardness, diametral tensile strength, flexural strength and modulus of elasticity. Moreover, these results are better than the parameters characterizing the composite containing the CQ/DMAEMA system. In terms of an aesthetic composite containing 0.75 wt.%. TPO is less yellow in color than the composite containing CQ/DMAEMA. This conclusion was objectively confirmed by test CIE L* a* b*.