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3D printing of materials which combine fracture toughness, high modulus and high strength is quite challenging. Most commercially available 3D printing resins contain a mixture of multifunctional (meth)acrylates. The resulting 3D printed materials are therefore brittle and not adapted for the preparation of denture bases. For this reason, this article focuses on toughening by incorporation of triblock copolymers in methacrylate-based materials. In a first step, three urethane dimethacrylates with various alkyl spacer length were synthesized in a one-pot two-step synthesis. Each monomer was combined with 2-phenoxyethyl methacrylate as a monofunctional monomer and a polycaprolactone-polydimethylsiloxane-polycaprolactone triblock copolymer was added as toughener. The formation of nanostructures via self-assembly was proven by small angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). The addition of the triblock copolymer resulted in a strong increase in fracture toughness for all mixtures. The nature of the urethane dimethacrylate had a significant impact on fracture toughness and flexural strength and modulus of the cured materials. Most promising systems were also investigated via dynamic fatigue propagation da/dN measurements, confirming that the toughening also works under dynamic load. By carefully selecting the length of the urethane dimethacrylate spacer and the amount of block copolymer, materials with the desired physical properties could be efficiently formulated. Especially the formulation containing the medium alkyl spacer length (DMA2/PEMA) and 5 wt% BCP1 (block copolymer), exhibits excellent mechanical properties and high fracture toughness., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Aim: This study aimed to synthesize and characterize a novel Bis -GMA analog, termed P- Bis -GMA, through structural modification by replacing hydroxyl (-OH) groups with phosphonooxy [-O-P(=O)(OH) 2 ] groups and to evaluate and compare its viscosity with Bis -GMA., Materials and Methods: Bis -GMA, triethylamine, dichloromethane, and phosphoryl chloride were utilized for the synthesis of P- Bis -GMA through phosphorylation. Fourier discerned the chemical structure of the synthesized P- Bis -GMA transform infrared spectroscopy (FTIR), and its viscosity was assessed by rheometry in oscillatory shear mode over a frequency sweep range of 0.1-100 (ω, rad/s) at 25°C with a 25 mm parallel plate design and a 0.5 mm gap. The data was recorded and statistically analyzed., Results: The FTIR analysis confirmed the successful synthesis of P- Bis -GMA, evidenced by the disappearance of hydroxyl (-OH) peaks and the emergence of phosphonooxy [-O-P(=O)(OH) 2 ] peaks in the P- Bis -GMA. Rheological testing demonstrated a notable reduction in viscosity for P- Bis -GMA (436.62 Pa.s) when compared to conventional Bis -GMA (1089.02 Pa.s), indicating improved handling characteristics., Conclusion: P- Bis -GMA was successfully synthesized by phosphorylation reaction where the -OH groups responsible for the high viscosity in the Bis -GMA were replaced with the [-O-P(=O)(OH) 2 ] groups with significantly reduced viscosity., Clinical Significance: The development of P- Bis -GMA holds promise for simplifying dental procedures by reducing chairside time with uncooperative children. The P-Bis -GMA-based composites possess self-adhering properties thereby eschewing the etching and bonding procedures with reduced moisture contamination of the restoration during bonding. This ultimately leads to better clinical outcomes and improved patient experiences by reducing technical vulnerabilities. How to cite this article: Ajay R, Selvabalaji A, Muthamilselvi M, et al. Synthesis and Characterization of a Chemico-structurally Modified Bis-GMA Analog for Dental Applications. J Contemp Dent Pract 2024;25(6):588-592.

Objective: Bisphenol A glycidyl methacrylate (Bis-GMA) is of great importance for dental materials as the preferred monomer. However, the presence of bisphenol-A (BPA) core in Bis-GMA structure causes potential concerns since it is associated with endocrine diseases, developmental abnormalities, and cancer lesions. Therefore, it is desirable to develop an alternative replacement for Bis-GMA and explore the intrinsic relationship between monomer structure and resin properties., Methods: Here, the betulin maleic diester derivative (MABet) was synthesized by a facile esterification reaction using plant-derived betulin and maleic anhydride as raw materials. Its chemical structure was confirmed by 1 H and 13 C NMR spectra, FT-IR spectra, and HR-MS, respectively. The as-synthesized MABet was then used as polymerizable comonomer to partially or completely substitute Bis-GMA in a 50:50 Bis-GMA: TEGDMA resin (5B5T) to formulate dental restorative resins. These were then determined for the viscosity behavior, light transmittance, real-time degree of conversion, residual monomers, mechanical performance, cytotoxicity, and antibacterial activity against Streptococcus mutans (S. mutans) in detail., Results: Among all experimental resins, increasing the MABet concentration to 50 wt% made the resultant 5MABet5T resin have a maximum in viscosity and appear dark yellowish after polymerization. In contrast, the 1MABet4B5T resin with 10 wt% MABet possessed comparable shear viscosity and polymerization conversion (46.6 ± 1.0% in 60 s), higher flexural and compressive strength (89.7 ± 7.8 MPa; 345.5 ± 14.4 MPa) to those of the 5B5T control (48.5 ± 0.6%; 65.7 ± 6.7 MPa; 223.8 ± 57.1 MPa). This optimal resin also had significantly lower S. mutans colony counts (0.35 ×10 8 CFU/mL) than 5B5T (7.6 ×10 8 CFU/mL) without affecting cytocompatibility., Significance: Introducing plant-derived polymerizable MABet monomer into dental restorative resins is an effective strategy for producing antibacterial dental materials with superior physicochemical property., Competing Interests: Declaration of Competing Interest We hereby confirm that all of the authors have read this manuscript, and no related work is in the press with any other journal. There are no known potential conflicts of interest with this work., (Copyright © 2024 Elsevier Inc. All rights reserved.)

Periodontitis is a common infectious disease characterized by loss of tooth-supporting structures, which eventually leads to tooth loss. The heavy burden of periodontal disease and its negative consequence on the patient's quality of life indicate a strong need for developing effective therapies. According to the World Health Organization, 10⁻15% of the global population suffers from severe periodontitis. Advances in understanding the etiology, epidemiology and microbiology of periodontal pocket flora have called for antibacterial therapeutic strategies for periodontitis treatment. Currently, antimicrobial strategies combining with polymer science have attracted tremendous interest in the last decade. This review focuses on the state of the art of antibacterial polymer application against periodontal pathogens and biofilms. The first part focuses on the different polymeric materials serving as antibacterial agents, drug carriers and periodontal barrier membranes to inhibit periodontal pathogens. The second part reviews cutting-edge research on the synthesis and evaluation of a new generation of bioactive dental polymers for Class-V restorations with therapeutic effects. They possess antibacterial, acid-reduction, protein-repellent, and remineralization capabilities. In addition, the antibacterial photodynamic therapy with polymeric materials against periodontal pathogens and biofilms is also briefly described in the third part. These novel bioactive and therapeutic polymeric materials and treatment methods have great potential to inhibit periodontitis and protect tooth structures.

Objective: A novel copper-bearing titanium alloy (Ti-Cu) was fabricated for dental application that is expected to efficiently restrain the growth of bacteria and discourage biofilm formation. The aim of this study was to investigate both the antibacterial activity and biofilm inhibition of Ti-Cu alloy in vitro, and the antibacterial effect of Ti-Cu implant in early stage of peri-implantitis in vivo., Methods: Staphylococcus aureus and Escherichia coli were selected to evaluate the antibacterial activity of Ti-Cu alloy and Ti served as control. The antibacterial rate, attached bacteria and developed biofilms were studied from quantitative antibacterial test, biofilm observation and bacterial morphological examination. Electrochemical tests were used to investigate the corrosion property of Ti-Cu alloy. Furthermore, both Ti and Ti-Cu dental implants were manufactured and then implanted in the mandibular premolar sites of beagle dogs for 3 months with ligature-infected treatment. Implant-tissue samples were prepared for radiographic analysis, Micro-CT evaluation and histological examination., Results: Ti-Cu alloy was found to efficiently kill the attached bacteria by ways of damaging cell membranes and cell walls and strongly inhibit the biofilm formation. However, Ti-Cu alloy had excellent corrosion resistance similar with Ti. Further, Ti-Cu dental implants showed superior capacities of inhibiting the bone resorption caused by bacterial infection and enhancing bone formation., Significance: Ti-Cu alloy strongly inhibited biofilm formation in vitro and prevented bacterial infection associated with dental implant in vivo, making it great potential for application in dental implants with excellent antibacterial viability and positive effect against bone resorption induced by peri-implantitis., (Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.)

Objective: To fabricate and characterise a novel biomimetic composite material consisting of aligned porous ceramic preforms infiltrated with polymer., Method: Freeze-casting was used to fabricate and control the microstructure and porosity of ceramic preforms, which were subsequently infiltrated with 40-50% by volume UDMA-TEGDMA polymer. The composite materials were then subjected to characterisation, namely density, compression, three-point bend, hardness and fracture toughness testing. Samples were also subjected to scanning electron microscopy and computerised tomography (Micro-CT)., Results: Three-dimensional aligned honeycomb-like ceramic structures were produced and full interpenetration of the polymer phase was observed using micro-CT. Depending on the volume fraction of the ceramic preform, the density of the final composite ranged from 2.92 to 3.36g/cm 3 , compressive strength ranged from 206.26 to 253.97MPa, flexural strength from 97.73 to 145.65MPa, hardness ranged from 1.46 to 1.62GPa, and fracture toughness from 3.91 to 4.86MPam 1/2 ., Significance: Freeze-casting provides a novel method to engineer composite materials with a unique aligned honeycomb-like interpenetrating structure, consisting of two continuous phases, inorganic and organic. There was a correlation between the ceramic fraction and the subsequent, density, strength, hardness and fracture toughness of the composite material., (Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.)

Cyanoacrylate adhesives and their homologues have elicited interest over the past few decades owing to their applications in the biomedical sector, extending from tissue adhesives to scaffolds to implants to dental material and adhesives, because of their inherent biocompatibility and ability to polymerize solely with moisture, thanks to which they adhere to any substrate containing moisture such as the skin. The ability to tailor formulations of alkyl cyanoacrylate to form derivative compounds to meet application requirements along with their biodegradability in conjunction with their inherent biocompatibility make them highly sought after candidates in the biomedical sector. There has been extensive exploration of cyanoacrylate adhesives and their homologue systems in biomedical applications, but no consolidated literature of the vast data is available. The ability of cyanoacrylate adhesives to cure at low temperatures and without the need for any hardener, which is attributed to the high-strength bonding interaction between two non-amalgamating substrates, with their ease of dispersion and self-curing, avoids the curtailing of the effective utilization of such adhesives in biomedical engineering applications as bio glues for amalgamating tissues, implants, scaffolds etc. This article consolidates copious work on cyanoacrylate adhesives and their derived systems which are functional in versatile biomedical engineering applications such as bio glues, dental material and adhesives and other potential applications.

Several new urethane-based dimethacrylates were synthesized, characterized and used to formulate the resin composites. Compressive strength (CS) was used as a screen tool to evaluate the mechanical property of the formed composites. Flexural strength, diametral tensile strength, water sorption, degree of conversion and shrinkage of the composites were also evaluated. The results show that most of the synthesized urethane-based dimethacrylates were solid, which are not suitable to dental filling restorations. However, it was found that liquid urethane-based dimethacrylates could be derivatized using asymmetrical methacrylate synthesis. Not only the newly synthesized urethane-based dimethacrylates showed lower viscosity values but also their constructed composites exhibited higher mechanical strengths. Without triethyleneglycol dimethacrylate (TEGDMA) addition, the new urethane-constructed composites showed significantly lower water sorption and shrinkage.

Objectives: This study describes the synthesis of brushite nanoparticles (CaHPO 4 ·2H 2 O) functionalized with triethylene glycol dimethacrylate (TEGDMA) and their application in dental restorative composites with remineralizing capabilities., Methods: Nanoparticles were synthesized, with TEGDMA being added to one of the precursor solutions at three different molar ratios (0:1, 0.5:1 and 1:1, in relation to the ammonium phosphate precursor). Then, they were added (10 vol%) to a photocurable dimethacrylate matrix containing 50 vol% of reinforcing glass particles. The resulting composites were tested for degree of conversion, biaxial flexural strength and elastic modulus (after 24h and 28days in water), and ion release (over a 28-day period). Commercial composites (one microhybrid and one microfilled) were tested as controls., Results: The final TEGDMA content in the functionalizing layer was modulated by the molar ratio added to the precursor solution. Functionalization reduced nanoparticle size, but did not reduce agglomeration. Improved mechanical properties were found for the composite containing nanoparticles with higher TEGDMA level in comparison to the composite containing non-functionalized nanoparticles or those with a low TEGDMA level. All brushite composites presented statistically significant reductions in strength after 28 days in water, but only the material with high-TEGDMA nanoparticles retained strength similar to the microhybrid commercial control. Overall, ion release was not affected by functionalization and presented steady levels for 28 days., Significance: Though agglomeration was not reduced by functionalization, the improvement in the matrix-nanoparticle interface allowed for a stronger material, without compromising its remineralizing potential., (Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.)

Objective: Two leading causes contributing to dental restoration replacement are the marginal breakdown at the composite/dentin interface and secondary caries mediated by bacteria. The objective of the present study was to synthesize oligomers which incorporated enhanced bio-stability but would also be able to generate antimicrobial function if they underwent degradation., Methods: Stability was incorporated into the oligomers by generating structural features that would physically hinder the availability of hydrolytically sensitive groups in the oligomers. As a proof-of concept for the antibacterial feature, antimicrobial function was achieved by covalently incorporating Ciprofloxacin (CF) into the backbone of cross-linking divinyl oligomers (referred to as EDV and HLH-CFPEG). The hydrolytic stability of the oligomers was studied in simulated human salivary esterase and compared to the commercial monomer 2,2-bis[4(2-hydroxy-3-methacryloxypropoxy)-phenyl]propane (BisGMA)., Results: Both drug oligomers were found to be significantly more stable than BisGMA. Upon degradation, both drug oligomers released CF differentially in free form. Polymer synthesis from resin formulations containing 15wt% HLH-CFPEG showed a high degree of vinyl group conversion and gel content, and under hydrolytic conditions showed the release of CF during a 28-day monitoring study period., Significance: HLH-CFPEG can be used in dental resin adhesive systems for local delivery of CF to the marginal interface. Minimizing the growth of Streptococcus mutans at the marginal site can improve longevity by reducing esterase activity derived specifically from S. mutans., (Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.)

Objective: The aim was to evaluate the effect of short glass-fiber/filler particles proportion on fracture toughness (FT) and flexural strength (FS) of an experimental flowable fiber-reinforced composite (Exp-SFRC) with two methacrylate resin formulations. In addition, we wanted to investigate how the fracture-behavior of composite restorations affected by FT values of SFRC-substructure., Methods: Exp-SFRC was prepared by mixing 50wt% of dimethacrylate based resin matrix (bisGMA or UDMA based) to 50wt% of various weight fractions of glass-fiber/particulate filler (0:50, 10:40, 20:30, 30:20, 40:10, 50:0wt%, respectively). FT and FS were determined for each experimental material following standards. Specimens (n=8) were dry stored (37°C for 2 days) before they were tested. Four groups of posterior composite crowns (n=6) composed of different Exp-SFRCs as substructure and surface layer of commercial particulate filler composite were fabricated. Crowns were statically loaded until fracture. Failure modes were visually examined. The results were statistically analysed using ANOVA followed by post hoc Tukey's test., Results: ANOVA revealed that ratio of glass-fiber/particulate filler had significant effect (p<0.05) on tested mechanical properties of the Exp-SFRC with both monomer systems. Exp-SFRC (50wt%) had significantly higher FT (2.6MPam 1/2 ) and FS (175.5MPa) (p<0.05) compared to non-reinforced material (1.3MPam 1/2 , 123MPa). Failure mode analysis of crown restorations revealed that FT value of the substructure directly influenced the failure mode., Significance: This study shows that short glass-fibers can significantly reinforce flowable composite resin and the FT value of SFRC-substructure has prior importance, as it influences the crack arresting mechanism., (Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

The objective of this study was to investigate several physicochemical properties of an experimental discontinuous S2-glass fiber-reinforced resin composite. The experimental composite was prepared by mixing 10 wt% of discontinuous S2-glass fibers with 27.5 wt% of resin matrix and 62.5 wt% of particulate fillers. Flexural strength (FS) and modulus (FM), fracture toughness (FT), work of fracture (WOF), double bond conversion (DC), Vickers hardness, volume shrinkage (VS) and fiber length distribution were determined. These were compared with two commercial resin composites. The experimental composite showed the highest FS, WOF and FT compared with two control composites. The DC of the experimental composite was comparable with controls. No significant difference was observed in VS between the three tested composites. The use of discontinuous glass fiber fillers with polymer matrix and particulate fillers yielded improved physical properties and substantial improvement was associated with the use of S2-glass fiber.

Objective: Investigate physical and chemical properties of model composites formulated with quaternary ammonium salt monomers (QAS) at different concentrations and alkyl chains lengths METHODS: QAS with 12 dimethylaminododecyl methacrylate (DMADDM) and 16 dimethylaminohexadecyl methacrylate (DMAHDM) chains lengths were synthesized and incorporated at 5 and 10% in model composites, resulting in four groups: G12.5 (DMADDM 5%), G12.10 (DMADDM 10%), G16.5 (DMAHDM 5%), G16.10 (DMAHDM 10%). One group was used as control group (CG 0%). Degree of conversion (DC); water sorption (WS) and solubility (SL); hygroscopic expansion (HE); degradation temperature (DT); glass transition temperature (T g ) and polymerization shrinkage (PS) were determined. Knoop hardness (KNH), flexural strength (FS) and elastic modulus (EM) were measured before and after storage Data were submitted to ANOVA and Tukey's test (p≤0.05)., Results: DC ranged between 76.1 (G12.10) and 70.7 (G16.5) %; CG had the lowest WS, SL and HE. There was no statistical difference for PS and FS. KHN values ranged between 30.2 (GC) and 25 (G16.10) and after storage the performance was depended on QAS concentration and chain length. For EM, CG had the highest values before and after storage and no difference was observed in the QAS groups before storage. After storage, the results were dependent on QAS concentration (3.5-4.3GPa)., Significance: In general, the addition of QAS increased composite's degradation compared with the CG. In the tested QAS, the addition of DMADDM at 5% concentration resulted in a less degradable material., (Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Four types of phosphorylated 2-hydroxyethyl methacrylate and poly(ethylene glycol) methyl ether methacrylate (PEGMA) block copolymers were synthesized by reversible addition fragmentation chain transfer (RAFT) polymerization and post-phosphorylation. These polymers were composed of different phosphate segments and similar PEG brushes. Polymers with defined phosphate segments were investigated to determine the optimal bonding affinity to hydroxyapatite (HAp). Polymers containing short phosphate segments (as low as 23 mer) were capable of immobilizing on HAp surfaces in situ in a short coating time with considerable durability. After surface modification, the dense PEG brushes altered the interfacial properties of HAp. The protein adsorption on the polymer-grafted HAp was drastically reduced compared with the bare HAp. Furthermore, the presence of the PEG brushes on the HAp surface resulted in bacterial inhibition. The polymer with the shortest phosphate segment (23 mer) showed superior inhibition ability., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Objective: Development of antibacterial dental composites is the ultimate goal to decrease carious disease occurrence and increase the restoration longevity. For this purpose, the quaternary ammonium dimethyl-hexadecyl-methacryloxyethyl-ammonium iodide (DHMAI) and the methacryloyloxyethylphosphorylcholine (MPC) have been incorporated in experimental methacrylate-based composite resins. This aims to first investigate the effect of each alone and then their combined effect., Methods: Synthesized DHMAI and commercial MPC were added either alone or combined at different concentrations to experimental dental composite. Flexural strength (FS) and modulus (FM) were tested to select the optimal concentrations. Only selected composites were evaluated for Vickers hardness (HV) and the degree of conversion (DC) using fourier transform infrared spectroscopy analysis (FTIR-ATR). Antibacterial activity was assessed using tests on colony-forming unit (CFU), scanning electron microscopy (SEM) and Alamarblue assay to measure the metabolic activity. Streptococcus mutans biofilm was chosen to be grown on the composite surfaces during 96h at 37°C., Results: Incorporation of 7.5% DHMAI in composite improved the degree of conversion and gave a strong antibacterial effect with a reduction of (∼98%) in CFU and (∼50%) of metabolic activity with acceptable mechanical properties. Addition of MPC to DHMAI affects mechanical properties of composites without providing a better antibacterial activity., Significance: Composites with DHMAI greatly reduced S. mutans biofilm and improved the degree of conversion without scarifying the composites' mechanical properties. DHMAI may have wide applicability to other dental materials in order to inhibit caries and improve the longevity of restorations., (Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

The aim of the study was to evaluate the influence of composite type and adhesive system on the quality of marginal adaptation in standardized Class V cavities before and after thermo-mechanical loading (TML). The cavities were restored using different combinations of three adhesive systems [(Silorane System Adhesive (SSA), Clearfil S 3 Bond (S3), G-Bond (G-B)] and two resin composite materials (Filtek Silorane, Clearfil AP-X). Six groups (n = 10): Group A (SSA-Primer + SSA-Bond, Filtek Silorane), Group B (SSA-Primer + SSA-Bond, Clearfil AP-X), Group C (S3 + SSA-Bond, Filtek Silorane), Group D (S3 + SSA-Bond, Clearfil AP-X), Group E (G-B + SSA-Bond, Filtek Silorane) and Group F (G-B + SSA-Bond, Clearfil AP-X) were defined. Marginal adaptation was assessed on replicas in the SEM at 200 × magnification before and after TML (3000 × 5-55 °C, 1.2 10 6  × 49 N; 1.7 Hz) under simulated dentinal fluid. The highest scores of continuous margins (%CM) were observed in the group F (G-B + SSA-Bond, Clearfil AP-X: before loading 96.4 (±3.2)/after loading 90.8 (±7.0)). A significant effect of adhesive system, composite type and loading interval was observed on the results (p < 0.05). Significantly lower scores of %CM were observed for silorane-based composite (Filtek Silorane) after TML in comparison with methacrylate-based composite (Clearfil AP-X) considering total marginal length (p < 0.05). For both Filtek Silorane and Clearfil AP-X, G-Bond performed significantly better than SSA-Primer and Clearfil S 3 Bond (p < 0.05). For all combinations of one-step self-etch adhesives and SSA-Bond resin coating, silorane-based low-shrinking composite exhibited inferior marginal adaptation than did the methacrylate-based composite.

Objective: In this study, we designed and synthesized a novel macromolecule (tetramethyl bisphenol F acrylate, TMBPF-Ac) with low viscosity, excellent mechanical properties, and good biocompatibility. It could be used as a monomer for dental resin composites, which could reduce the risk of human exposure to bisphenol A derivatives in the oral environment. In addition, the monomer could be used without diluent, thereby avoiding the negative effect of a diluent METHODS: TMBPF-Ac was synthesized by a multistep condensation reaction. Its structure was confirmed by 1 H NMR spectra. Different resin mixtures were prepared, and then a number of performance and cytotoxicity tests were performed on these specimens., Results: 1 H NMR spectra showed that the structure of TMBPF-Ac was in accordance with the design. The viscosity of TMBPF-Ac was obviously lower than that of bisphenol-A diglycidyl methacrylate. The three kinds of resins used in this study were in line with ISO 4049:2009 and ISO 10993-5:2009. TMBPF-Ac-based resin had better physical and biological properties., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The aim of this study was to synthesize and characterize new multifunctional-urethane-methacrylate monomers to be used as the organic matrix in restorative dental composites, and evaluate the main physical-chemical properties of the resulting material. Bis-GMA (bisphenol-A-diglycidylmethacrylate) and GDMA (glycerol dimethacrylate) were modified by reacting the hydroxyl groups with isocyanate groups of urethane-methacrylate precursors to result in the new monomeric systems U-(bis-GMA)-Mod and U-(GDMA)-Mod, U=Urethane and Mod=Modified. The modifications were characterized by FTIR and 1 H NMR. The final monomeric synthesized system was used to prepare dental resins and composites. The physical-chemical properties were evaluated and compared with those of bis-GMA composites with varying filler contents or unfilled resins. U-(bis-GMA)-Mod and U-(GDMA)-Mod can be used to prepare dental restorative composites, with some foreseeable advantages compared with bis-GMA composites. One significant advantage is that these composites have the potential to be less toxic, once they presented a reduction of 50% in leaching of unreacted monomers extracted by solvent., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Purpose: High purity, fine crystalline, degradation-free at low temperature powders have attracted special interest in CAD/CAM prosthetic dentistry full ceramic restorations. This study reports the preparation and characterisation of zirconia-ceria (0.9 ZrO2 0.1 CeO2) powders. Materials were obtained from zirconium-n-alkoxide and cerium nitrate hexahydrate in the pH 2-4 and 8-10., Methods: Zirconia- ceria powders were obtained with the sol-gel method in a humid-free environment. Thermal analysis (TGA/DTA) of the as-prepared materials was made for an assessment of its behaviour at elevated temperatures. Specimens were dried at 80 °C and calcinated in two stages: at 300 °C with soaking time 2.5 h and 850 °C with holding time 2.5 h, in order to evaluate the phase transformations. Thermal analyses of the as-dried powders were made for an assessment of its thermal behaviour during heat treatment up to 1000 °C. By X-ray diffraction (XRD), polymorphs of ZrO2 were identified. Additionally, scanning electron microscopy (SEM) and laser particle size distribution (PSD) were involved for characterisation of morphology of the powders., Results: A correlation between the pH of the colloidal system and the morphology of the as-obtained powders were found. Based on analysis (SEM, PSD), structures were identified known as soft and hard agglomerates., Conclusions: It can be stated that differences found between powder morphology were dependent on the value pH used, which can be crucial for powder densification during sintering and compacting green bodies which, as a consequence, may be crucial for the lifetime of zirconia prostheses. Correlations between phase composition and pH are difficult to grasp, and require further, more sophisticated, studies.

Purpose: The purpose of the study was to evaluate corrosion resistance of Wirobond C® alloy after chemical passivation treatment., Methods: The alloy surface undergone chemical passivation treatment in four different media. Corrosion studies were carried out by means of electrochemical methods in saline solution. Corrosion effects were determined using SEM., Results: The greatest increase in the alloy polarization resistance was observed for passive layer produced in Na2SO4 solution with graphite. The same layer caused the highest increase in corrosion current. Generally speaking, the alloy passivation in Na2SO4 solution with graphite caused a substantial improvement of the corrosion resistance. The sample after passivation in Na2SO4 solution without graphite, contrary to others, lost its protective properties along with successive anodic polarization cycles. The alloy passivation in Na3PO4 solution with graphite was the only one that caused a decrease in the alloy corrosion properties. The SEM studies of all samples after chemical passivation revealed no pit corrosion - in contrast to the sample without any modification., Conclusions: Every successive polarization cycle in anodic direction of pure Wirobond C® alloy enhances corrosion resistance shifting corrosion potential in the positive direction and decreasing corrosion current value. The chemical passivation in solutions with low pH values decreases susceptibility to electrochemical corrosion of Co-Cr dental alloy. The best protection against corrosion was obtained after chemical passivation of Wirobond C® in Na2SO4 solution with graphite. Passivation with Na2SO4 in solution of high pH does not cause an increase in corrosion resistance of WIROBOND C. Passivation process increases alloy resistance to pit corrosion.

With the aim of reducing human exposure to Bisphenol A (BPA) derivatives in dentistry, a fluorinated dimethacrylate monomer was synthesized to replace 2,2-bis[4-(2-hydroxy-3-methacryloy-loxypropyl)-phenyl]propane (Bis-GMA) as the base monomer of dental resin. After mixing with reactive diluent triethyleneglycol dimethacrylate (TEGDMA), fluorinated dimethacrylate (FDMA)/TEGDMA was prepared and compared with Bis-GMA/TEGDMA in physicochemical properties, such as double bond conversion (DC), volumetric shrinkage (VS), water sorption (WS) and solubility (WSL), flexural strength (FS) and modulus (FM). The results showed that, when compared with Bis-GMA based resin, FDMA-based resin had several advantages, such as higher DC, lower VS, lower WS, and higher FS after water immersion. All of these revealed that FDMA had potential to be used as a substitute for Bis-GMA. Of course, many more studies, such as biocompatibility testing, should be undertaken to prove whether FDMA could be applied in clinic., Competing Interests: The authors declare no conflict of interest.

Background: Resin-based dental materials allow bacterial growth on their surface and lack antibacterial activity, leading to functional and esthetic failure. Quaternary ammonium polyethyleneimine (QPEI) nanoparticles (NPs) incorporated in resin-based composite at 2% wt/wt have demonstrated prolonged and complete inhibition of bacterial growth. This study focused on optimization of QPEI NP synthesis to reduce the concentration required for bacterial growth inhibition. The objective here was to enhance antimicrobial efficacy by excess base neutralization, using phosphoric or hydrochloric acid, and by using surfactants., Methods: QPEI NP variants were prepared (i) under controlled neutralization of acid, using NaHCO3, (ii) under controlled carbonate ion neutralization with HCl or H3PO4 and (iii) by treatment with N-lauroylsarcosine or glycerol monostearate. NPs incorporated in the dental materials were examined for their antibacterial effect against Enterococcus faecalis., Results: Controlled addition of NaHCO3 resulted in modified QPEI NPs with an increased ability to inhibit bacterial growth. Surface treatment with N-lauroylsarcosine resulted in enhanced antibacterial activity at 0.5% wt/wt concentration in acrylate and epoxy resin-based dental materials., Conclusions: The antimicrobial efficacy of QPEI NP may be improved significantly by controlling the addition of NaHCO3, neutralization of excess base and the surface-agent effect.

Objective: To characterise and compare the tensile characteristics after multi-proportional blending, to determine the proper blending ratio for new thermoplastic material and to compare its mechanical performance with commercial thermoplastics., Methods: PETG and PC2858 aggregates were blended in five different ratios. Standard specimens of each ratio were molded and tested to determine their mechanical performance. Then the new material with the proper blending ratio was chosen and compared against commercial thermoplastics., Results: With the increase of PC2858 content, the tensile and impact strength increased but elongation at break decreased. When blending ratio (wt %) was 70/30, the PETG/PC2858 exhibited optimal mechanical properties, with a tensile strength of 63.42 ± 1.67 MPa, and a stress relaxation rate of 0.0080 ± 0.0005 N/s, which exceeded those of Erkodur and Biolon., Conclusion: By blending PETG and PC2858 at the weight ratio 70/30, we obtained new thermoplastic material which outperformed commercial products.

Objective: Bulk fracture is one of the primary reasons for resin-based dental restoration failures. To date, there has been no report on the use of polymerizable dental monomers with acceptable biocompatibility to develop a resin with substantial self-healing capability. The objectives of this study were to: (1) develop a self-healing resin containing microcapsules with triethylene glycol dimethacrylate (TEGDMA)-N,N-dihydroxyethyl-p-toluidine (DHEPT) healing liquid in poly(urea-formaldehyde) (PUF) shells for the first time, and (2) determine the physical and mechanical properties, self-healing efficiency, and fibroblast cytotoxicity., Methods: Microcapsules of polymerizable TEGDMA-DHEPT in PUF were prepared via an in situ polymerization method. Microcapsules were added into a BisGMA-TEGDMA resin at microcapsule mass fractions of 0%, 5%, 10%, 15% and 20%. A flexural test was used to measure composite strength and elastic modulus. A single edge V-notched beam method was used to measure fracture toughness KIC and self-healing efficiency., Results: Flexural strength and elastic modulus (mean±sd; n=6) of resin containing 5-15% microcapsules were similar to control without microcapsules (p>0.1). Adding microcapsules into the resin increased the virgin KIC, which was about 40% higher at 15% microcapsules than that with 0% microcapsules (p<0.05). Specimens were fractured and healed, then fractured again to measure the healed KIC. A self-healing efficiency of about 65% in KIC recovery was obtained with 10-20% microcapsules. All specimens with 0-20% microcapsules had fibroblast viability similar to control without resin eluents (p>0.1)., Significance: Self-healing dental resin containing microcapsules with polymerizable TEGDMA-DHEPT healing liquid in PUF shells were prepared for the first time with excellent self-healing capability. These microcapsules and self-healing resins containing them may be promising for dental restorations to heal cracks/damage and increase durability., (Copyright © 2015 Academy of Dental Materials. All rights reserved.)

Hydroxyapatite (HA), the main mineral component of bones and teeth, was synthesized by using the reaction between calcium nitrate tetrahydrate Ca(NO3)2∙4H2O and diammonium hydrogen phosphate (NH4)2HPO4 (DAHP) with a chemical precipitation method. The objective of this study is to utilize novel inorganic-organic nanocomposites for biomedical applications. HA is an inorganic component (75% w) and chitosan, alginate and albumin (Egg white) are organic components of nanocomposites (25% w). Nanocomposites were prepared in deionized water solutions, at room temperature, using a mechanical and magnetic stirrer for 48 h. The microstructure and morphology of sintered n-HAP were tested at different preheating temperature and laser sintering speed with scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR).

In this study, novel, quaternary ammonium methacrylate-modified silica nanoparticles (QMSNs) were synthesized for the first time and proposed as possible antimicrobial particles for free-radical, photocurable monomers. Such monomers have the potential to polymerize with other methacrylate monomers and create antimicrobial polymers. The silica nanoparticles were modified by quaternary ammonium methacrylate functionality and incorporated at 0 to 10 wt% into a 1:1 (by mass) bisphenol A glycerolate dimethacrylate (BisGMA)/triethylene glycol dimethacrylate (TEGDMA) resin. Thermal stability of the pristine and modified silica nanoparticles was examined by thermogravimetric analyses. Atomic force microscopy was used to investigate the size distribution and topography of the nanoparticles. For evaluation of the mechanical properties of the samples, flexural strength was measured using a 3-point bending test method. The flexural strength of the composites containing QMSNs increased with increasing modified silica content. The antimicrobial activity of samples was investigated against some standard microorganisms (Streptococcus mutans, Staphylococcus aureus, Bacillus subtilis, Escherichia coli, Pseudomonas aeruginosa, and Candida albicans), and then cytotoxicity and viability were quantified. Incorporation of 2.5% to 10% (by mass) QMSNs into BisGMA/TEGDMA demonstrated antimicrobial activity, but ≥5 wt% significantly reduced cell viability., (© International & American Associations for Dental Research 2015.)

Objective: Ceramic composites are promising materials for dental restorations. However, it is difficult to prepare highly translucent composites due to the light scattering that occurs in multiphase ceramics. The objective of this work was to verify the effectiveness of a systematic approach in designing specific glass compositions with target properties in order to prepare glass infiltrated ceramic composites with high translucency., Methods: First it was necessary to calculate from literature data the viscosity of glass at the infiltration temperature using the SciGlass software. Then, a glass composition was designed for targeted viscosity and refractive index. The glass of the system SiO2-B2O3-Al2O3-La2O3-TiO2 prepared by melting the oxide raw materials was spontaneously infiltrated into porous alumina preforms at 1200°C. The optical properties were evaluated using a refractometer and a spectrophotometer. The absorption and scattering coefficients were calculated using the Kubelka-Munk model., Results: The light transmittance of prepared composite was significantly higher than a commercial ceramic-glass composite, due to the matching of glass and preform refractive indexes which decreased the scattering, and also to the decrease in absorption coefficient., Significance: The proposed systematic approach was efficient for development of glass infiltrated ceramic composites with high translucency, which benefits include the better aesthetic performance of the final prosthesis., (Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

In clinic, it calls for effective and simple materials to repair etched dentin. Bioinspired by the natural mineralization process guided by noncollagenous proteins (NCPs), in this work, we synthesized the fourth generation phosphate-terminated polyamidoamine dendrimer (G4-PO3H2) by one-step modification. We used FT-IR and 1H NMR to characterize the structure of G4-PO3H2, and MTT assay to prove its biocompatibility. It was applied as the analog of dentin phosphophoryn (DPP: a type of NCPs) to repair dentin, due to its similar dimensional scale, topological architecture and peripheral functionalities to that of DPP. By the characterization of SEM and XRD, the effective regeneration of human dentin induced by G4-PO3H2 is characterized and illustrated both in vitro (artificial saliva) and in vivo (oral cavity of rats). It is noted that the thickness of the regenerated mineral layers are more than 10 μm both in vitro and in vivo. The design strategy of G4-PO3H2 may be valuable for researchers in the fields of material science, stomatology and medicine to prepare various promising restorative nano-materials for biomineralized hard tissues such as bone and teeth., (Copyright © 2015 Elsevier B.V. All rights reserved.)

The aim of the present study was to investigate the effects of a composite nanofibrous matrix made of biopolymer blend polycaprolactone-gelatin (BP) and mesoporous bioactive glass nanoparticles (BGNs) on the odontogenic differentiation of human dental pulp cells (HDPCs). BGN-BP nanomatrices, with BGN content of up to 20 wt%, were produced via electrospinning. The differentiation of the HDPCs was evaluated by using an ALP activity assay, calcified nodule formation, and mRNA expression for markers. Integrin and its underlying signal pathways were assessed via reverse transcriptase-polymerase chain reaction and Western blot analysis. Although cell growth and attachment on the BGN-BP nanomatrix was similar to that on BP, ALP activity, mineralized nodule formation, and mRNA, expressions involving ALP, osteocalcin, osteopontin, dentin sialophosphoprotein, and dentin matrix protein-1 were greater on BGN-BP. BGN-BP upregulated the key adhesion receptors (integrin components α1, α2, α5, and β1) and activated integrin downstream pathways, such as phosphorylated-focal adhesion kinase (p-FAK), and p-paxillin. In addition, BGN-BP activated BMP receptors, BMP-2 mRNA, and p-Smad 1/5/8, and such activation was blocked by the BMP antagonist, noggin. Furthermore, BGN-BP induced phosphorylation of extracellular signal-regulated kinase, protein kinase 38, and c-Jun-N-terminal kinase mitogen-activated protein kinases and activated expression of the transcription factors Runx2 and Osterix in HDPCs. Collectively, the results indicated for the first time that a BGN-BP composite nanomatrix promoted odontogenic differentiation of HDPCs through the integrin, BMP, and mitogen-activated protein kinases signaling pathway. Moreover, the nanomatrix is considered to be promising scaffolds for the culture of HDPCs and dental tissue engineering., (© The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.)

Purpose: The aim of this study was to compare the residual monomer and microhardness of poly(methyl methacrylate) (PMMA)-based denture resins processed by using autoclave and conventional water bath techniques., Methods: To determine the amount of residual methyl methacrylate (MMA) monomer, disk-shaped specimens (n=5) were prepared from 3 different acrylic resins (Meliodent, Paladent and Qc-20). Control groups were polymerized in water bath for 30 minutes at 100°C. The study groups were prepared in an autoclave device for 60°C/30 min followed 130°C/10 min and the other group for 60°C/30 min followed by 130°C/20 min. According to standard calibration curves, ultraviolet spectrophotometry at 230 nm was used to determine the residual monomer. For the Vickers hardness measurements, disk-shaped specimens (n=5) were prepared for each test group. Hardness measurements were performed with a Vickers hardness tester under a 4.91-N press load for a 30 seconds, after immersion in distilled water at 37ºC for 48 hours. The data were analyzed by ANOVA and Tukey HSD test (p<0.05)., Results: Autoclave polymerization produced a significant decrease in the amount of residual monomers for all resin groups (p<0.05). This procedure also showed a significant increase in hardness for all resin groups (p<0.05). For the 3 resin groups, no significant differences were found between autoclave polymerization for 10 minutes and for 20 minutes (p>0.05)., Conclusions: The autoclave polymerization technique exhibited significantly lower residual monomer content and greater hardness than conventional heat polymerization.

Dental professionals are seeing a growing population of patients with visible signs of dental erosion. The approach currently being used to address the problem typically leverages the enamel protection benefits of fluoride. In this report, an alternative new block copolymer with a hydrophilic polyacrylic acid (PAA) block and a hydrophobic poly(methyl methacrylate) (PMMA) block was developed to similarly reduce the mineral loss from enamel under acidic conditions. This series of PMMA-b-PAA block copolymers was synthesized by reversible addition fragmentation transfer (RAFT) polymerization. Their structures were characterized by gel permeation chromatography (GPC) and (1)H nuclear magnetic resonance (NMR) spectra. The molar fractions of acrylic acid (AA) in the final block copolymer were finely controlled from 0.25 to 0.94, and the molecular weight (Mn) of PMMA-b-PAA was controlled from 10 kDa to 90 kDa. The binding capability of the block copolymer with hydroxyapatite (HAP) was investigated by ultraviolet-visible spectroscopy (UV-Vis) and Fourier transform infrared (FTIR) spectroscopy. FTIR spectra confirmed that the PMMA-b-PAA block copolymer could bind to HAP via bridging bidentate bonds. Both UV-Vis and FTIR spectra additionally indicated that a high polymer concentration and low solution pH favored the polymer binding to HAP. The erosion-preventing efficacy of the PMMA-b-PAA block copolymer in inhibiting HAP mineral loss was quantitatively evaluated by atomic absorption spectroscopy (AAS). Based on the results, polymer treatment reduced the amount of calcium released by 27% to 30% in comparison with the unprotected samples. Scanning electron microscope (SEM) observations indicated that PMMA-b-PAA polymer treatment protected enamel from acid erosion. This new amphiphilic block copolymer has significant potential to be integrated into dentifrices or mouthrinses as an alternative non-fluoride ingredient to reduce tooth erosion., (© International & American Associations for Dental Research.)

Polymeric dental adhesives require the formation of densely crosslinked network structures to best ensure mechanical strength and durability in clinical service. Monomeric precursors to these materials typically consist of mixtures of hydrophilic and hydrophobic components that potentially undergo phase separation in the presence of low concentrations of water, which is detrimental to material performance and has motivated significant investigation into formulations that reduce this effect. We have investigated an approach to network formation based on nanogels that are dispersed in inert solvent and directly polymerized into crosslinked polymers. Monomers of various hydrophilic or hydrophobic characteristics were copolymerized into particulate nanogels bearing internal and external polymerizable functionality. Nanogel dispersions were stable at high concentrations in acetone or, with some exceptions, in water and produced networks with a wide range of mechanical properties. Networks formed rapidly upon light activation and reached high conversion with extremely low volumetric shrinkage. Prepolymerizing monomers into reactive nanostructures significantly changes how hydrophobic materials respond to water compared with networks obtained from polymerizations involving free monomer. The modulus of fully hydrated networks formed solely from nanogels was shown to equal or exceed the modulus in the dry state for networks based on nanogels containing a hydrophobic dimethacrylate and hydrophilic monomethacrylate, a result that was not observed in a hydroxyethyl methacrylate (HEMA) homopolymer or in networks formed from nanogels copolymerized with HEMA. These results highlight the unique approach to network development from nanoscale precursors and properties that have direct implications in functional dental materials., (© International & American Associations for Dental Research.)

One of the leading causes for the failure of dental composite restorations is secondary caries. Effectively inhibiting cariogenic biofilms and reducing secondary caries could extend the service life of composite restorations. Dental composites releasing antibacterial agents such as chlorhexidine (CHX) have shown biofilm-inhibitory efficacy, but they usually have poor physical and mechanical properties. Herein, we present a study of a new method to encapsulate and release CHX from dental composite using mesoporous silica nanoparticles (MSNs). SBA-15 MSNs were synthesized according to a reported procedure. CHX (62.9 wt%) was encapsulated into dried MSN from 0.3 M CHX ethanol solution. The dental composites containing 0% (control), 3%, 5%, and 6.3% CHX or the same amounts of CHX entrapped in MSN (denoted as CHX@MSN) were fabricated with methacrylate monomers and silanized glass fillers (CHX or CHX@MSN + glass filler particle = 70 wt%). The monomer mixture consisted of bisphenol A glycidyl methacrylate (BisGMA), hexanediol dimethacrylate (HDDMA), ethoxylated bisphenol A dimethacrylate (EBPADMA), and urethane dimethacrylates (UEDMA) at a weight ratio of 40:30:20:10. The composites were tested for CHX release and recharge, flexural strength and modulus (at 24 hr and 1 mo), surface roughness, in vitro wear, and antibacterial activity against Streptococcus mutans and Lactobacillus casei (in both planktonic growth and biofilm formation). The results showed that the composites with CHX@MSN largely retained mechanical properties and smooth surfaces and showed controlled release of CHX over a long time. In contrast, the composites with directly mixed CHX showed reduced mechanical properties, rough surfaces, and burst release of CHX in a short time. The composites with CHX either directly mixed or in MSN showed strong inhibition to S. mutans and L. casei. This research has demonstrated the successful application of MSNs as a novel nanotechnology in dental materials to inhibit oral biofilm without sacrificing materials' mechanical properties and surface integrity., (© International & American Associations for Dental Research.)

Adult orthodontics is recently gaining popularity due to its importance in esthetics, oral and general health. However, none of the currently available alumina or zirconia based ceramic orthodontic brackets meet the esthetic demands of adult patients. Inherent hexagonal lattice structure and associated birefringence limits the visible light transmission in polycrystalline alumina and make them appear white and non transparent. Hence focus of the present study was to assess the feasibility of using magnesium aluminate (MgAl2O4) spinel; a member of the transparent ceramic family for esthetic orthodontic brackets. Transparent spinel specimens were developed from commercially available white spinel powder through colloidal shaping followed by pressureless sintering and hot isostatic pressing at optimum conditions of temperature and pressure. Samples were characterized for chemical composition, phases, density, hardness, flexural strength, fracture toughness and optical transmission. Biocompatibility was evaluated with in-vitro cell line experiments for cytotoxicity, apoptosis and genotoxicity. Results showed that transparent spinel samples had requisite physico-chemical, mechanical, optical and excellent biocompatibility for fabricating orthodontic brackets. Transparent spinel developed through this method demonstrated its possibility as a prospective biomaterial for developing esthetic orthodontic brackets.

There is an increasing clinical need to design novel dental materials that combine regenerative and antibacterial properties. In this work the characterization of a recently developed sol-gel-derived bioactive glass ceramic containing silver ions (Ag-BG) is presented. The microstructural characteristics, ion release profile, zeta potential value and changes in weight loss and pH value as a function of the immersion time of Ag-BG in Tris buffer are evaluated. Ag-BG is also incorporated into natural extracellular matrix (ECM) hydrogel to further enhance its regenerative properties. Then, the micro and macro architectures of these new composites (ECM/Ag-BG) are characterized. In addition, the antibacterial properties of these new composites are tested against Escherichia coli and Enterococcus faecalis, a bacterium commonly implicated in the pathogenesis of dental pulp infections. Cell-material interaction is also monitored in a primary culture of dental pulp cells. Our study highlights the benefits of the successful incorporation of Ag in the bioactive glass, resulting in a stable antibacterial material with long-lasting bactericidal activity. Furthermore, this work presents for the first time the fabrication of new Ag-doped composite materials, with inductive pulp-cell proliferation and antibacterial properties (ECM/Ag-BG). This advanced composite made of Ag-BG incorporated into natural ECM possesses improved properties that may facilitate potential applications in tooth regeneration approaches., (Copyright © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.)

In this paper we describe the one-pot fabrication of hydroxyapatite (HA)-heparin composites by electrodeposition onto Ti substrates and their characterisation in terms of structure, morphology, heparin content and bioactivity. HA coatings are well known and widely applied osteointegration enhancers, but post-implant healing rate in dental applications is still suboptimal: e.g. coagulation control plays a key role and the incorporation of an anticoagulant is considered a highly desirable option. In this study, we have developed an improved, simple and robust growth procedure for single-phase, pure HA-heparin films of thickness 1/3 μm. HA-heparin, forming nanowires, has the ideal morphology for bone mineralisation. Staining assays revealed homogeneous incorporation of sizable amounts of heparin in the composite films. The bioactivities of the HA and HA-heparin coatings on Ti were compared by HeLa cell proliferation/viability tests and found to be enhanced by the presence of the anticoagulant.

This works reports a set of new functionalized polyethyleneimine (PEI) polymers, including a neutral PEGylated polymer PEI-g-PEGMA, a negatively charged polymer PEI-g-SA, and a zwitterionic polymer PEI-g-SBMA, and their use as antibiofouling coating agent for human teeth protection. Polymers were synthesized by Michael addition, XPS analysis revealed that each polymer could be efficiently coated onto hydroxyapatite, ceramic material used as a model tooth. Polymers carrying a negative net charge were more efficiently adsorbed, because of the establishment of electrostatic interactions with calcium ions. Protein adsorption tests revealed that two factors were important in the reduction of protein adsorption. Both the surface charge and the surface ability to bind and entrap water molecules had to be considered. PEI-g-SBMA, which zeta potential in PBS solution was negative, was efficient to inhibit the adsorption of BSA, a negative protein. On the other hand, it also resisted the adsorption of lysozyme, a positive protein, because zwitterionic molecules can easily entrap water and provide a very hydrophilic environment. Streptococcus mutans attachment tests performed unveiled that all modified polymers were efficient to resist this type of bacteria responsible for dental carries. Best results were also obtained with PEI-g-SBMA coating. This polymer was also shown to efficiently resist the adsorption of positively charged bacteria (Stenotrophomonas maltophilia). Tests performed on real human tooth showed that PEI-g-SBMA could inhibit up to 70% of bacteria adhesion, which constitutes a major result considering that surface of teeth is very rough, therefore physically promoting the attachment of proteins and bacteria.

Introduction: This investigation aimed to assess and compare the amount of residual monomer (RM) released from removable orthodontic appliances constructed by sprinkle-on and dough techniques., Materials and Methods: One hundred and twenty acrylic samples were prepared from orthodontic autopolymerized acrylic resins and divided into three groups, according to the processing method: sprinkle-on with polyclave, sprinkle-on without polyclave and dough technique. After polymerization, the specimens of each group were immersed in distilled water for 24 h, 48 h, 72 h and 1 week. High-performances liquid chromatography (HPLC) was utilized to measure residual monomer content., Results: Maximum observed RM was 1284·91±129·07 ppm measured for sprinkle-on technique without polyclave after 24 h of water immersion. At this time, the level of RM was significantly different among the three applied techniques (P<0·05). In all soaking time groups, sprinkle-on technique with polyclave released the least amount of RM. Within each group, the maximum monomer releasing was observed after the first 24 h and decreases were observed in subsequent time groups. The reduction over the time was not significant in the polyclave groups (P>0·05)., Conclusion: The sprinkle-on technique with polyclave and longer water immersion reduced residual monomer released from acrylic orthodontic appliances.

With growing concern over bacterial resistance, the identification of new antimicrobial means is paramount. In the oral cavity microorganisms are essential to the development of periradicular diseases and are the major causative factors associated with endodontic treatment failure. As quaternary ammonium compounds have the ability to kill a wide array of bacteria through electrostatic interactions with multiple anionic targets on the bacterial surface, it is likely that they can overcome bacterial resistance. Melding these ideas, we investigated the potency of a novel endodontic sealer in limiting Enterococcus faecalis growth. We used a polyethyleneimine scaffold to synthesize nano-sized particles, optimized for incorporation into an epoxy-based endodontic sealer. The novel endodontic sealer was tested for its antimicrobial efficacy and evaluated for biocompatibility and physical eligibility. Our results show that the novel sealer foundation affixes the nanoparticles, achieving surface bactericidal properties, but at the same time impeding nanoparticle penetration into eukaryotic cells and thereby mitigating a possible toxic effect. Moreover, adequate physical properties are maintained. The nanosized quaternary amine particles interact within minutes with bacteria, triggering cell death across wide pH values. Throughout this study we demonstrate a new antibacterial perspective for endodontic sealers; a novel antibacterial, effective and safe antimicrobial means.

Objectives: Composites are the principal material for tooth cavity restorations due to their esthetics and direct-filling capabilities. However, composites accumulate biofilms in vivo, and secondary caries due to biofilm acids is the main cause of restoration failure. The objectives of this study were to: (1) synthesize new antibacterial monomers and (2) develop nanocomposite containing nanoparticles of amorphous calcium phosphate (NACP) and antibacterial monomer., Methods: Two new antibacterial monomers were synthesized: dimethylaminohexane methacrylate (DMAHM) with a carbon chain length of 6, and dimethylaminododecyl methacrylate (DMADDM) with a chain length of 12. A spray-drying technique was used to make NACP. DMADDM was incorporated into NACP nanocomposite at mass fractions of 0%, 0.75%, 1.5%, 2.25% and 3%. A flexural test was used to measure composite strength and elastic modulus. A dental plaque microcosm biofilm model with human saliva as inoculum was used to measure viability, metabolic activity, and lactic acid production of biofilms on composites., Results: The new DMAHM was more potent than a previous quaternary ammonium dimethacrylate (QADM). DMADDM was much more strongly antibacterial than DMAHM. The new DMADDM-NACP nanocomposite had strength similar to that of composite control (p>0.1). At 3% DMADDM in the composite, the metabolic activity of adherent biofilms was reduced to 5% of that on composite control. Lactic acid production by biofilms on composite containing 3% DMADDM was reduced to only 1% of that on composite control. Biofilm colony-forming unit (CFU) counts on composite with 3% DMADDM were reduced by 2-3 orders of magnitude., Significance: New antibacterial monomers were synthesized, and the carbon chain length had a strong effect on antibacterial efficacy. The new DMADDM-NACP nanocomposite possessed potent anti-biofilm activity without compromising load-bearing properties, and is promising for antibacterial and remineralizing dental restorations to inhibit secondary caries., (Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Objectives: To synthesize and characterize machinable, bioactive glass-ceramics (GCs) suitable for dental implant applications., Methods: A glass in the SiO2-Al2O3-CaO-CaF2-K2O-B2O3-La2O3 system was synthesized by wet chemical methods, followed by calcination, melting and quenching. Crystallization kinetics were determined by differential thermal analysis (DTA). GC discs were produced by cold pressing of the glass powder and sintered using schedules determined by DTA. The crystalline phases and microstructure of GC samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Dynamic Young's modulus (E), true hardness (Ho), fracture toughness (KIC) and brittleness index (BI) were evaluated. Bioactivity was studied by examining the formation of hydroxyapatite (HA) on the GC surfaces after soaking in simulated body fluid (SBF). Attachment and proliferation of MC3T3-E1 osteoblastic cells were assessed in vitro., Results: Miserite [KCa5(Si2O7)(Si6O15)(OH)F] was the main crystalline phase of the GC with additional secondary phases. Microstructural studies revealed interlocking lath-like crystalline morphology. E, Ho, and KIC values for the GCs were 96±3 GPa, 5.27±0.26 GPa and 4.77±0.27 MPa m(0.5), respectively. The BI was found to be 1.11±0.05 μm(-0.5), indicating outstanding machinability. An HA surface layer was formed on the GC surfaces when soaked in SBF, indicating potential bioactivity. MC3T3-E1 cells exhibited attachment, spreading and proliferation on GC surfaces, demonstrating excellent biocompatibility., Significance: We present a novel approach for the synthesis of miserite GC with the physical and biological properties required for non-metallic dental implant applications., (Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.)

Dental caries, also known as tooth decay or a cavity, remains a major public health problem in the most communities even though the prevalence of disease has decreased since the introduction of fluorides for dental care. Therefore, biomaterials to fill dental defects appear to be necessary to fulfill customers' needs regarding the properties and the processing of the products. Bioceramics and glass-ceramics are widely used for these purposes, as dental inlays, onlays, veneers, crowns or bridges. Calcium orthophosphates belong to bioceramics but they have some specific advantages over other types of bioceramics due to a chemical similarity to the inorganic part of both human and mammalian bones and teeth. Therefore, calcium orthophosphates (both alone and as components of various formulations) are used in dentistry as both dental fillers and implantable scaffolds. This review provides brief information on calcium orthophosphates and describes in details current state-of-the-art on their applications in dentistry and dentistry-related fields. Among the recognized dental specialties, calcium orthophosphates are most frequently used in periodontics; however, the majority of the publications on calcium orthophosphates in dentistry are devoted to unspecified "dental" fields.

The selective laser melting (SLM) process was applied to a Co-29Cr-6Mo alloy, and its microstructure, mechanical properties, and metal elution were investigated to determine whether the fabrication process is suitable for dental applications. The microstructure was evaluated using scanning electron microscopy with energy-dispersed X-ray spectroscopy (SEM-EDS), X-ray diffractometry (XRD), and electron back-scattered diffraction pattern analysis. The mechanical properties were evaluated using a tensile test. Dense builds were obtained when the input energy of the laser scan was higher than 400 J mm⁻³, whereas porous builds were formed when the input energy was lower than 150 J mm⁻³. The microstructure obtained was unique with fine cellular dendrites in the elongated grains parallel to the building direction. The γ phase was dominant in the build and its preferential <001> orientation was confirmed along the building direction, which was clearly observed for the builds fabricated at lower input energy. Although the mechanical anisotropy was confirmed in the SLM builds due to the unique microstructure, the yield strength, UTS, and elongation were higher than those of the as-cast alloy and satisfied the type 5 criteria in ISO22764. Metal elution from the SLM build was smaller than that of the as-cast alloy, and thus, the SLM process for the Co-29Cr-6Mo alloy is a promising candidate for fabricating dental devices., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

To reduce the polymerization shrinkage of the dental resin composites, a new liquid-crystalline resin monomer was developed. The acrylate liquid crystalline resin monomer (ALCRM), (4-3-(acryloyloxy)-2-hydroxypropoxy) phenyl 4-(3-(acryloyloxy)-2-hydroxypropoxy) benzoate, was synthesized by a three-step method. Using the ALCRM as the main monomer, the degree of conversion (DC) and the volume shrinkage of the resin matrix were compared with the traditional composite resin monomer (Bis-GMA), 2,2-bis[4-(2-hydroxy-3-methacryloyloxy-propoxy)-phenyl] propane. The new monomer showed liquid crystalline characteristics with a mesomorphic phasetransition temperature between 18ºC and 42ºC. When copolymerized with triethylene glycol dimethacrylate (TEGDMA) at a weight ratio of 7:3, the DC of ALCRM was higher and the volume shrinkage was 3.62±0.26%, which was less than that of the Bis-GMA. The ALCRM exhibits promising potential for the development of superior dental resins with low volume shrinkage.

The investigation of titanium (Ti) surface modifications aiming to increase implant osseointegration is one of the most active research areas in dental implantology. This study was carried out to evaluate the benefits of coating Ti with type I collagen on the osseointegration of dental implants. Acid etched Ti implants (AETi), either untreated or coated with type I collagen (ColTi), were placed in dog mandibles for three and eight weeks for histomorphometric, cellular and molecular evaluations of bone tissue response. While the histological aspects were essentially the same with both implants being surrounded by lamellar bone trabeculae, histomorphometric analysis showed more abundant bone formation in ColTi, mainly at three weeks. Cellular evaluation showed that cells harvested from bone fragments in close contact with ColTi display lower proliferative capacity and higher alkaline phosphatase activity, phenotypic features associated with more differentiated osteoblasts. Confirming these findings, molecular analyses showed that ColTi implants up-regulates the expression of a panel of genes well known as osteoblast markers. Our results present a set of evidences that coating AETi with collagen fastens the osseointegration by stimulating bone formation at the cellular and molecular levels, making this combination of morphological and biochemical modification a promising approach to treat Ti surfaces.

The aim of this work was to synthesize and investigate properties of a novel dimethacrylic monomer based on bioderived alicyclic diol--isosorbide. Its potential as a possible substitute of 2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)phenyl]propane (BISGMA), widely used in dental restorative materials and suspected for toxicity was assessed. The novel monomer was obtained in a three-step synthesis. First, isosorbide was etherified by a Williamson nucleophilic substitution and subsequently oxidized to isosorbide diglycidyl ether (ISDGE). A triphenyl phosphine catalyzed addition of methacrylic acid to ISDGE resulted in 2,5-bis(2-hydroxy-3-methacryloyloxypropoxy)- 1,4:3,6-dianhydro-sorbitol (ISDGMA). The monomer obtained was photopolymerized using camphorquinone/2-(dimethylamino)ethyl methacrylate initiating system. Next, compositions with triethylene glycol dimethacrylate (TEGDMA) were prepared and polymerized. Double bond conversion, polymerization shrinkage and water sorption of resulting polymers were determined. Selected mechanical (flexular strength and modulus, Brinell hardness) and thermomechanical (DMA analysis) properties were also investigated. BISGMA based materials were prepared as reference for comparison of particular properties.

The purpose of this study was to investigate the use of different plasticizers in soft acrylic resin materials to reduce leaching of the plasticizer and thus increase the durability of tissue conditioners. Samples were prepared containing different combinations of three types of polymer/copolymer powder and four types of plasticizer liquid (DEHM, DIBA, DAA and DINA). The dynamic viscoelasticity of each sample was measured after water immersion using a dynamic mechanical analyzer. Water absorption, solubility and weight change were also measured. A significant difference was found among the materials regarding dynamic viscoelasticity, water absorption and solubility. The samples containing P-n-BMA had the most stable G' and G'' scores throughout the immersion. P-n-BMA is the most suitable powder together with DEHM as the most suitable liquid component for a tissue conditioner. These results suggest that it is possible to improve the durability of tissue conditioners by combining different polymers and plasticizers.

Objectives: The widespread incidence of recurrent caries highlights the need for improved dental restorative materials. The objective of this study was to synthesize low viscosity ionic dimethacrylate monomers (IDMAs) that contain quaternary ammoniums groups (antimicrobial functionalities) and are compatible with existing dental dimethacrylate-based monomers. Such monomers have the potential to copolymerize with other methacrylate monomers and produce antibacterial polymers., Methods: Two monomers (IDMA-1 and IDMA-2) were synthesized using the Menschutkin reaction and incorporated at 0-30% (by mass) into a 1:1 (by mass) bisphenol A glycerolate dimethacrylate (BisGMA):triethylene glycol dimethacrylate (TEGDMA) resin. Resin viscosity was quantified using rheology, and polymer degree of conversion (DC) and surface charge density were measured using Fourier transform infrared spectroscopy (FTIR) and fluorescein binding, respectively. Effects of IDMA-1 on initial attachment of Streptococcus mutans and on viability and metabolic activity (via reductase enzymes) of RAW 264.7 macrophage-like cells were quantified., Results: IDMA-1 and IDMA-2 were prepared and characterized. IDMA-1 was miscible with BisGMA:TEGDMA and slightly increased the resin viscosity and DC. As expected, polymeric surface charge density increased with increasing IDMA-1. Incorporation of 10% IDMA-1 into BisGMA:TEGDMA reduced bacterial colonization without affecting viability or metabolic activity of mammalian cells. Increasing IDMA-1 up to 30% had no additional effect on bacterial coverage, but ≥20% IDMA-1 significantly reduced macrophage density, viability, and metabolic activity. Leachables from polymers containing IDMA-1 were not cytotoxic., Significance: The Menschutkin reaction provides a facile, convenient means to synthesize new monomers with quaternary ammonium groups for dental and medical applications., (Published by Elsevier Ltd.)

Background: Inhibition of Candida albicans on denture resins could play a significant role in preventing the development of denture stomatitis. The safety of a new dental material with antifungal properties was analyzed in this work., Methods: Poly(methyl methacrylate) [PMMA] discs and PMMA-silver nanoparticle discs were formulated, with the commercial acrylic resin, Nature-Cryl™, used as a control. Silver nanoparticles were synthesized and characterized by ultraviolet-visible spectroscopy, dispersive Raman spectroscopy, and transmission electron microscopy. The antifungal effect was assessed using a luminescent microbial cell viability assay. Biocompatibility tests were carried out using NIH-3T3 mouse embryonic fibroblasts and a Jurkat human lymphocyte cell line. Cells were cultured for 24 or 72 hours in the presence or absence of the polymer formulations and analyzed using three different tests, ie, cellular viability by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay, and cell proliferation by enzyme-linked immunosorbent assay BrdU, and genomic DNA damage (Comet assay). Finally, the samples were evaluated mechanically, and the polymer-bearing silver nanoparticles were analyzed microscopically to evaluate dispersion of the nanoparticles., Results: The results show that PMMA-silver nanoparticle discs significantly reduce adherence of C. albicans and do not affect metabolism or proliferation. They also appear not to cause genotoxic damage to cells., Conclusion: The present work has developed a new biocompatible antifungal PMMA denture base material.

In this study, hydrogels composed of polyethyleneimine (PEI) and poly(vinyl pyrrolidone) K90 (PVP) cross-linked with various concentrations (0, 0.125, 0.25 and 0.5%) of glutaraldehyde were evaluated as a hydrogel filler for the local delivery of lidocaine after tooth extraction. The drug-release kinetics, swellability, cytotoxicity and wound healing after tooth extraction of these non-cross-linked and cross-linked PEI-PVP hydrogels were examined in male beagles and compared to values using Spongostan(®). Results demonstrated that the extent of cross-linking influenced the swelling of the resulting hydrogel, but the drug-release rates were similar. No significant changes were observed in gingival fibroblasts in contact with the PEI- PVP hydrogels or Spongostan(®). In the in vivo study, PEI-PVP hydrogels showed good retention in the socket for 2 days and showed comparable wound-healing rates within 2 weeks with those of Spongostan(®). In conclusion, PEI-PVP hydrogels are suitable for use as socket-dressing materials, and the release of local anaesthesia from PEI-PVP hydrogels can be sustained for a desirable period of time to prevent pain after a tooth extraction.