A novel low shrinkage dimethacrylate monomer as an alternative to BisGMA for adhesive and resin-based composite applications.

The aim of this study was to develop a mixture of dimethacrylate isomers (PG6EMA) as a potential monomer for dental adhesives and composites. PG6EMA was synthesized de novo and characterized in the presence of ethanol (3%, 6% or 9%). BisGMA/TEGDMA (BTEG, 50/50 wt.%) was used as the resin control. Composites were formulated with 60 wt.% of either PG6EMA or BisGMA (40 wt.% TEGDMA and 70 wt.% filler). DMPA (0.2 wt.%) and DPI-PF6 (0.4 wt.%) were added as photoinitiators, irradiated with a mercury arc lamp (320-500 nm, 500 mW/cm2; Acticure). All materials were tested for polymerization kinetics (near-infrared), viscosity (η) and storage modulus (G', oscillatory rheometry). The composites were further characterized for water sorption/solubility, wet/dry flexural strength/modulus and polymerization stress. Data were analyzed with one-way ANOVA/Tukey's test (α = 0.05). The PG6EMA resins showed lower rates of polymerization compared with BTEG (p = 0.001) but high degrees of conversion (p = 0.002). Solvent concentration did not affect RPMAX but the 6% and 9% mixtures showed higher final DC, likely due to reduced viscosity. PG6EMA had much higher viscosity than BTEG (p <0.001) and lower G' (p = 0.003). Composites modified with PG6EMA have slower polymerization rates (p = 0.001) but higher final DC (p = 0.04) than the control. PG6EMA/TEGDMA showed lower dry/wet flexural strength and comparable dry modulus. The PG6EMA/TEGDMA composite showed a 18.4% polymerization stress reduction compared to the BTEG composite. Both base monomers had similar WS/SL and G'. Within its limitations, this study demonstrated that the newly synthesized PG6EMA was a viable alternative to BisGMA in dental composites.

Effect of replacing Bis-GMA with a biobased trimethacrylate on the physicochemical and mechanical properties of experimental resin composites.

OBJECTIVES: To analyze the incorporation of cardanol trimethacrylate monomer (CTMA), derived from the cashew nut shell liquid, as a substitute for Bis-GMA in acrylic resins formulations and its effect on experimental resin composites' physicochemical and mechanical properties. MATERIALS AND METHODS: The intermediary cardanol epoxy was synthesized via cardanol epoxidation, followed by the synthesis of CTMA through methacrylic anhydride solvent-free esterification. Experimental resin composites were formulated with an organic matrix composed of Bis-GMA/TEGDMA (50/50 wt %) (control). CTMA was gradually added to replace different proportions of Bis-GMA: 10 wt % (CTMA-10), 20 wt % (CTMA-20), 40 wt % (CTMA-40), and 50 wt % (CTMA-50). The composites were characterized by degree of conversion, water sorption and solubility, viscosity, thermogravimetric analysis, dynamic mechanical analysis, flexural strength and elastic modulus. Data were analyzed with one-way ANOVA and Tukey's post-hoc test (α = 0.05), except for water sorption data, which were analyzed by Kruskall-Wallis and Dunn's method. RESULTS: CTMA-based and control composites did not show statistically significant differences regarding degree of conversion, flexural strength and elastic modulus. CTMA reduced the viscosity and solubility compared to the Bis-GMA-based composite. The CTMA-40 and CTMA-50 exhibited significantly lower water sorption compared to the control. Also, acceptable thermal stability and viscoelastic properties were obtained for safe use in the oral cavity. CONCLUSIONS: Incorporating CTMA into composites resulted in similar chemical and mechanical properties compared to Bis-GMA-based material while reducing viscosity, water sorption and solubility. CLINICAL RELEVANCE: CTMA could be used as a trimethacrylate monomer replacing Bis-GMA in resin composites, thereby minimizing BPA exposure.

Physicochemical properties of flowable composites using isobornyl methacrylate as diluent monomer.

OBJECTIVE: this study sought to evaluate the effect of isobornyl methacrylate (IBOMA) as a diluent monomer on the physicochemical properties of experimental flowable resin composites. METHODOLOGY: the organic resin matrix of a modal flowable resin composite was formulated with 50 wt.% of bisphenol-A-glycidyl methacrylate (Bis-GMA) and 50 wt.% of a diluent monomer, in which IBOMA was used as a combining or substituent diluent monomer to triethylene glycol dimethacrylate (TEGDMA). The resin matrices were filled with 55 wt.% particles, of which 10 wt.% was 0.05-µm fumed silica, and 45 wt.% was 0.7-µm BaBSiO2 glass. Polymerization shrinkage stress (PSS; n=10), degree of conversion (DC; n=3), maximum rate of polymerization (Rpmax; n=3), film thickness (FT; n=10), sorption (Wsp; n=10), solubility (Wsl; n=10), flexural strength (FS; n=10), flexural modulus (FM; n=10), Knoop microhardness (KH; n=10), and microhardness reduction after chemical softening (HR; n=10) were evaluated. Data were analyzed using one-way ANOVA, followed by Tukey's test (α=0.05; ß=0.2). RESULTS: the results showed that the substitution or addition of IBOMA reduced FT (p=0.001), PSS (p=0.013), Rpmax (p=0.001), DC (p=0.001), FM (p=0.006) Wsp (p=0.032), and Wsl (p=0.021). However, when used as a complete substituent, IBOMA demonstrated significantly lower FS (p=0.017) and KH (p=0.008), while TEGDMA demonstrated significantly lower HR (p=0.022). CONCLUSION: the flowable composite containing IBOMA combined with TEGDMA showed no effect in KH and FS and effectively reduced the PSS, RP, FT, Wsp, and Wsl. However, it showed a reduction in DC, FS, and an increase in HR.

Effect of adding ytterbium trifluoride filler particles on the mechanical, physicochemical and biological properties of methacrylate-based experimental resins for 3D printing.

OBJECTIVE: To formulate an experimental methacrylate-based photo-polymerizable resin for 3D printing with ytterbium trifluoride as filler and to evaluate the mechanical, physicochemical, and biological properties. METHODS: Resin matrix was formulated with 60 wt% UDMA, 40 wt% TEGDMA, 1 wt% TPO, and 0.01 wt% BHT. Ytterbium Trifluoride was added in concentrations of 1 (G1 %), 2 (G2 %), 3 (G3 %), 4 (G4 %), and 5 (G5 %) wt%. One group remained without filler addition as control (GC). The samples were designed in 3D builder software and printed using a UV-DLP 3D printer. The samples were ultrasonicated with isopropanol and UV cured for 60 min. The resins were tested for degree of conversion (DC), flexural strength, Knoop microhardness, softening in solvent, radiopacity, colorimetric analysis, and cytotoxicity (MTT and SRB). RESULTS: Post-polymerization increased the degree of conversion of all groups (p < 0.05). G2 % showed the highest DC after post-polymerization. G2 % showed no differences in flexural strength from the G1 % and GC (p > 0.05). All groups showed a hardness reduction after solvent immersion. No statistical difference was found in radiopacity, softening in solvent (ΔKHN%), colorimetric spectrophotometry, and cytotoxicity (MTT) (p > 0.05). G1 % showed reduced cell viability for SRB assay (p < 0.05). SIGNIFICANCE: It was possible to produce an experimental photo-polymerizable 3D printable resin with the addition of 2 % ytterbium trifluoride as filler without compromising the mechanical, physicochemical, and biological properties, comparable to the current provisional materials.

Physicochemical characterization of experimental resin-based materials containing calcium orthophosphates or calcium silicate.

OBJECTIVE: To evaluate experimental dimethacrylate-based materials containing calcium orthophosphates or calcium silicate particles in terms of their optical, mechanical and Ca2+ release behaviour. METHODS: Dicalcium phosphate dihydrate (DCPD), hydroxyapatite (HAp), beta-tricalcium phosphate (ß-TCP) or calcium silicate (CaSi) particles were added to a photocurable BisGMA/TEGDMA resin (1:1 in mols) at a 30 vol% fraction. Materials containing silanized or non-silanized barium glass particles were used as controls. Degree of conversion (DC) at the top and base of 2-mm thick specimens was determined by ATR-FTIR spectroscopy (n = 5). Translucency parameter (TP) and transmittance (%T) were determined using a spectrophotometer (n = 3). Biaxial flexural strength (BFS) and flexural modulus (FM) were determined by biaxial flexural testing after 24 h storage in water (n = 10). Ca2+ release in water was determined during 28 days by inductively coupled plasma optical emission spectrometry (n = 3). Statistical analysis was performed using ANOVA/Tukey test (DC: two-way; TP, %T; BFS and FM: one-way; Ca2+ release: repeated measures two-way, α = 5 %). RESULTS: CaSi and ß-TCP particles drastically reduced DC at 2 mm, TP and %T (p < 0.001). Compared to both controls, all Ca2+-releasing materials presented lower BFS (p < 0.001) and only the material with DCPD showed significantly lower FM (p < 0.05). The material containing CaSi presented the highest Ca2+ release, while among materials formulated with calcium orthophosphates the use of DCPD resulted in the highest release (p < 0.001). SIGNIFICANCE: CaSi particles allowed the highest Ca2+ release. Notwithstanding, the use of DCPD resulted in a material with the best compromise between optical behaviour, DC, strength and Ca2+ release.

Antimicrobial Composites Based on Methacrylic Acid-Methyl Methacrylate Electrospun Fibers Stabilized with Copper(II).

This study presents fibers based on methacrylic acid-methyl methacrylate (Eudragit L100) as Cu(II) adsorbents, resulting in antimicrobial complexes. Eudragit L100, an anionic copolymer synthesized by radical polymerization, was electrospun in dimethylformamide (DMF) and ethanol (EtOH). The electrospinning process was optimized through a 22-factorial design, with independent variables (copolymer concentration and EtOH/DMF volume ratio) and three repetitions at the central point. The smallest average fiber diameter (259 ± 53 nm) was obtained at 14% w/v Eudragit L100 and 80/20 EtOH/DMF volume ratio. The fibers were characterized using scanning electron microscopy (SEM), infrared spectroscopy in attenuated total reflectance mode (FTIR-ATR), and differential scanning calorimetry (DSC). The pseudo-second-order mechanism explained the kinetic adsorption toward Cu(II). The fibers exhibited a maximum adsorption capacity (qe) of 43.70 mg/g. The DSC analysis confirmed the Cu(II) absorption, indicating complexation between metallic ions and copolymer networks. The complexed fibers showed a lower degree of swelling than the non-complexed fibers. The complexed fibers exhibited bacteriostatic activity against Gram-negative (Pseudomonas aeruginosa) and Gram-positive (Staphylococcus aureus) bacteria. This study successfully optimized the electrospinning process to produce thin fibers based on Eudragit L100 for potential applications as adsorbents for Cu(II) ions in aqueous media and for controlling bacterial growth.

Achieving property enhancements in dental resin composites via reduced concentrations of camphorquinone within a ternary initiator system.

OBJECTIVES: The study aimed to assess the impact of diphenyliodonium hexafluorophosphate (DPI) on the physicochemical properties of experimental resin composites (ECRs) featuring reduced concentrations of camphorquinone (CQ)/amine. METHODS: Five concentrations of CQ (0.125, 0.25, 0.5, 0.75, and 1 mol%) with dimethylaminoethyl amine benzoate (EDAB) in a 1:2 mol% ratio (CQ:EDAB) were incorporated into a 50:50 mass% monomer blend of bisphenol glycidyl methacrylate (BisGMA) and triethyleneglycol dimethacrylate (TEGDMA). An additional 5 groups with the same CQ:EDAB concentrations had 0.5 mol% DPI added. Each resin group contained 60 wt% of 0.7 µm barium-alumino-silicate glass. Light transmission (n = 3), real-time degree of polymerization (n = 3), temperature change during polymerization (n = 5), polymerization shrinkage strain (n = 3), flexural strength, and modulus (n = 12), as well as water sorption and solubility (n = 5), were evaluated. Data were analyzed using two-way ANOVA and Tukey's post-hoc test (α = 0.05). RESULTS: Light transmission was reduced in groups containing 0.125 and 0.25 mol% of CQ without DPI. DPI increased temperature, degree and rate of polymerization, despite the reduction in CQ/amine concentration. Additionally, there was an increase in polymerization shrinkage strain, flexural strength and modulus, and a reduction in water sorption and solubility in ECRs with DPI, even with lower concentrations of CQ/EDAB. SIGNIFICANCE: DPI improved the assessed properties of composites across various concentrations of CQ/EDAB, showing the benefit of reducing the quantity of CQ used without compromising the properties and curing of the resin composites.

A new method of adhesive system application improves the bond strength between fiber post and root dentin.

This study evaluated a new method of adhesive system application on the bond strength between fiber post and root dentin using two adhesive systems. The canals of sixty bovine incisors were prepared and obturated. The roots were divided into six groups (n=10) according to the adhesive system (Clearfil SE - CSE and Single Bond Universal - SBU) and the application strategy (microbrush - MB; rotary brush - RB; and ultrasonic tip - US). The glass fiber posts were cemented with resin cement (RelyX ARC). The roots were sectioned perpendicularly to their long axis, and three slices per root were obtained. Previously to the push-out test, confocal laser scanning microscopy (CLSM) was performed to illustrate the interfacial adaptation of the cement to the root canal walls. Failure patterns were analyzed with 40x magnification. Shapiro-Wilk indicated a normal distribution of the data. The bond strength values were compared using one-way ANOVA and Tukey's tests. Student's T test analyzed the differences between the adhesive systems within each third and protocol. A significance level of 5% was used. CSE with RB showed higher mean bond strength values compared to MB (conventional technique) (P < 0.05). US application resulted in intermediate bond strength values for CSE (P > 0.05). The application of SBU using RB generated higher mean bond strength values compared to MB and US (P < 0.05). Adhesive failures were predominant (65.5%). CSE and SBU application with the new rotary brush improved the bond strength of fiber posts to root dentin compared to the conventional strategy.

The influence of filler load in 3D printing resin-based composites.

OBJECTIVE: To evaluate the influence of the barium glass (BG) filler in 3D printing resin-based composites for restorative structures. METHODS: Experimental 3D printing resin-based composites were formulated with UDMA 70%wt, Bis-EMA 20%wt, and TEGDMA 10%wt. Photoinitiators TPO and DFI (2%wt) were used. BG was incorporated at 40%wt and 50%wt. 0%wt BG was used as negative control and the VarseoSmile Crownplus (Bego) was used as a commercial control. Specimens were printed using a 3D printer. Subsequently, specimens were washed and submitted to post-curing with 405 nm at 60ºC for 2 × 20 min at FormCure (FormLabs). 3D printing resin-based composites were evaluated by flexural strength, degree of conversion, softening in solvent, radiopacity, and cytotoxicity against gingival fibroblasts. Data were statistically analyzed using one-way ANOVA (α = 0.05). RESULTS: No significant differences in flexural strength were showed between BG40% (90.5 ± 5,4 MPa), BG50% (102.0 ± 11.7 MPa) and VA (105.2 ± 11.7 MPa). Addition of 40% and 50% of BG showed no influence in the degree of conversion compared to VA (p > 0.05). All groups showed softening in solvent after immersion in ethanol (p < 0.05). All groups showed more than 1mmAl of radiopacity. BG50% showed significantly higher radiopacity (2.8 ± 0.3 mmAl) than other groups (p < 0,05). Cytotoxicity evaluation showed gingival cell viability higher than 80% for all groups. SIGNIFICANCE: Addition of up to 50%wt of barium glass in experimental 3D printing resin-based composites showed promising results for long-term restorative structures.

Ion release mechanisms in composites containing CaP particles and hydrophilic monomers.

OBJECTIVE: To investigate the effect of hydrophilic/permeable polymer matrices on water sorption/solubility (WS/SL), Ca2+ release, mechanical properties and hydrolytic degradation of composites containing dicalcium phosphate dihydrate (DCPD) particles. METHODS: Six composites were tested, all with 10 vol% of glass particles and either 30 vol% or 40 vol% DCPD. Composites containing 1BisGMA:1TEGDMA in mols (at both inorganic levels) were considered controls. Four materials were formulated where 0.25 or 0.5 of the BisGMA/TEGDMA was replaced by pyromellitic dianhydride glycerol dimethacrylate (PMGDM)/ polyethylene glycol dimethacrylate (PEGDMA). Composites were tested for degree of conversion (FTIR spectroscopy), WS/SL (ISO 4049) and Ca2+ release (inductively coupled plasma optical emission spectroscopy). Fracture toughness (FT) and biaxial flexural strength/modulus (BFS/FM) were determined after 24 h and 60 days in water. The contributions of diffusional and relaxational mechanisms to Ca2+ release kinetics were analyzed using the semi-empirical Salim-Peppas model. Data were analysed by ANOVA/Tukey test (alpha: 0.05). RESULTS: WS/SL was higher for composites containing PMGDM/PEGDMA compared to the controls (p < 0.001). Only at 40% DCPD the 0.5 PMGDM/PEGDMA composite showed statistically higher Ca2+ release than the control. Relaxation diffusion was the main release mechanism. Initial FT was not negatively affected by matrix composition. BFS (both DCPD fractions) and FM (30% DCPD) were lower for composites with hydrophilic/permeable networks (p < 0.01). After 60 days in water, composites with PMGDM/PEGDMA presented significant reductions in FT, while all composites had reductions in BFS/FM. SIGNIFICANCE: Increasing matrix hydrophilicity/permeability significantly increased Ca2+ release only at a high DCPD fraction.

Nano-in-nano enteric protein delivery system: coaxial Eudragit® L100-55 fibers containing poly(N-vinylcaprolactam) nanogels.

Oral protein delivery holds significant promise as an effective therapeutic strategy for treating a wide range of diseases. However, effective absorption of proteins faces challenges due to biological barriers such as harsh conditions of the stomach and the low permeability of mucous membranes. To address these challenges, this article presents a novel nano-in-nano platform designed for enteric protein delivery. This platform, obtained by electrospinning, involves a coaxial arrangement comprising poly(N-vinylcaprolactam) nanogels (NGs) enclosed within nanofibers of Eudragit® L100-55 (EU), a pH-responsive polymer. The pH-selective solubility of EU ensures the protection of NGs during their passage through the stomach, where the fibers remain intact at low pH, and releases them in the intestine where EU dissolves. The switchable characteristic of this nano-in-nano platform is confirmed by using NGs loaded with a model protein (ovalbumin), which is selectively released when the intestinal pH is achieved. The versatility of this nano-in-nano delivery platform is demonstrated by the ability to modify the fibers dissolution profile simply by adjusting the concentration of EU used in the electrospinning process. Furthermore, by tuning the properties of NGs, the potential applications of this platform can be further extended, paving the way for diverse therapeutic possibilities.

Effect of elastomeric urethane monomer on physicochemical properties and shrinkage stress of resin composites.

This study aimed to evaluate the effect of an elastomeric urethane monomer (Exothane-24) in different concentrations on physicochemical properties, gap formation, and polymerization shrinkage stress of experimental resin composites. All experimental composites were prepared with 50 wt.% of Bis-GMA and 50 wt.% of TEGDMA, to which 0 wt.% (control), 10 wt.%, 20 wt.%, 30 wt.%, and 40 wt.% of Exothane-24 were added. Filler particles (65 wt.%) were then added to these resin matrixes. Ultimate tensile strength (UTS: n = 10), flexural strength (FS: n = 10), flexural modulus (FM: n = 10), hardness (H: n = 10), hardness reduction (HR: n = 10), degree of conversion (DC: n = 5), gap width (GW: n = 10), and polymerization shrinkage stress in Class I (SS-I: n = 10) and Class II (SS-II: n = 10) simulated configuration. All test data were analyzed using one-way ANOVA and Tukey's test (α = 0.05;  = 0.2). Exothane-24 in all concentrations decreased the H, HR, DC, GW, SS-I, and SS-II (p < 0.05) without affecting the UTS, and FS (p > 0.05). Reduction in FM was observed only in the Exothane 40% and 30% groups compared to the control (p < 0.05). Exothane-24 at concentrations 20% and 30% seems suitable since it reduced GW and polymerization SS without affecting the properties of the composite resins tested, except for H.

Radiopacity and physical properties evaluation of infiltrants with Barium and Ytterbium addition.

Radiopaque properties in the infiltrant should be interesting for clinicians to feel more confident to indicate this treatment. Thus, the aim of this study was to evaluate the effect of the incorporation of barium and ytterbium particles on the physical properties of resin infiltrants. Groups were divided according to the addition of ytterbium oxide (Y) alone (30 or 40%) or Y with barium (YB) (15/15% or 20/20% respectively) in the Icon commercial infiltrant and in the experimental infiltrant base. Digital radiography (n=5), Microradiography (n=5), Microtomography (n=3), degree of conversion (n=5), water sorption (n=16), solubility (n=16), contact angle (n=16), flexural strength (n=16), elastic modulus (n=16) and Energy dispersive X-ray Spectroscopy (n=10) were performed. Analyses were performed using the R program, with a significance level of 5%, and microradiography and Microtomography analyses were evaluated qualitatively. In groups with 30 or 40% of ytterbium, radiopacity was higher or equal to enamel. Microradiography and Microtomography appear to have more radiopacity in groups with 40% (Y). Among the groups with no particle addition, those of the experimental infiltrant presented a higher degree of conversion than those of Icon®. In most groups, there was solubility below the ISO-recommended levels. The addition of particles resulted in higher viscosity. Groups with Icon had higher flexural strength and elastic modulus than groups with experimental infiltrant. The addition of 40% (Y) improved polymerization, had low solubility, and had greater radiopacity than enamel, however negatively affected the viscosity increasing then. Experimental groups with the base showed a higher water sorption than Icon groups.

Effect of preheating on mechanical properties of a resin-based composite containing elastomeric urethane monomer.

This study investigated the effect of preheating an elastomeric urethane monomer (Exothane-24) experimental resin composite on its physicochemical properties. Two resin matrices were formulated: (a) 50 wt% Bisphenol-glycidyl methacrylate (Bis-GMA) and 50 wt% triethylene glycol dimethacrylate (TEGDMA); and (b) 20 wt% Exothane-24, 40 wt% Bis-GMA and 40 wt% TEGDMA. A photoinitiator system (0.25 wt% camphorquinone and 0.50 wt% ethyl-4-dimethylamino benzoate) and 65 wt% of the inorganic filler (20 wt% 0.05 µm silica and 80 wt% 0.7 µm BaBSiO2 glass) were added to both matrices. These formulations were then assigned to four groups: Exothane-24 (E); Exothane-24 plus preheating (EH); no Exothane-24 (NE); and no Exothane-24 plus preheating (NEH). NEH and EH were preheated at 69 °C. The dependent variables were as follows: film thickness (FT); polymerization shrinkage stress (PSS); gap width (GW); maximum rate of polymerization (Rpmax); and degree of conversion (DC). Data were statistically analyzed by two-way ANOVA and Tukey's test (α = 0.05). Preheating reduced FT for both composites. PSS and GW were significantly lower for EH, when compared with E. The DC for EH and NEH and the Rpmax for EH increased significantly. Preheating improved most of the physicochemical properties (FT, PSS, GW, and DC) of the experimental resin composite containing Exothane-24.

Release of leachable products from resinous compounds in the saliva of children with anterior open bite treated with spur.

BACKGROUND: To evaluate the release of bisphenol-A glycidyl methacrylate (BisGMA), triethylene glycol dimethacrylate (TEGDMA), bisphenol A (BPA), and phthalates of the composite resin used in the bonding of spurs applied in the treatment of children with anterior open bite and its effects on human keratinocytes. METHODOLOGY: Saliva samples of 22 children were collected before spur attachment (baseline) and 30 minutes (min) and 24 hours (h) after spur bonding. Analysis was performed using high-performance liquid chromatography (HPLC) coupled to tandem mass spectrometry (HPLC-MS/MS) and gas chromatography coupled to mass spectrometry (GC-MS). Standardized resin increments were added to three different dilutions of the cell culture medium. Keratinocytes (HaCaT) were cultivated in the conditioned media and evaluated for cell viability (MTT) and cell scratch assay. RESULTS: The levels of BisGMA (1.74±0.27 µg/mL), TEGDMA (2.29±0.36 µg/mL), and BPA (3.264±0.88 µg/L) in the saliva after 30 min, in comparison to baseline (0±0 µg/mL, 0±0 µg/mL, and 1.15±0.21 µg/L, respectively), presented higher numbers. After 24 h, the levels of the monomers were similar to the baseline. Phthalates showed no significant difference among groups. HaCat cells showed increased viability and reduced cell migration over time after exposure to methacrylate-based resin composites. CONCLUSION: Resin composites, used to attach spurs in children with anterior open bite during orthodontic treatment, release monomers after polymerization and can influence the behavior of human keratinocytes, even at very low concentrations. Orthodontists should be aware of the risks of the resinous compounds release and preventive procedures should be held to reduce patient exposure.

Development of functional fillers as a self-healing system for dental resin composite.

OBJECTIVES: To evaluate the incorporation of repairing capsules containing different monomers and polymerization modulators on the self-healing efficiency of an experimental photopolymerizable resin-based composite. METHODS: Self-healing capsules containing different monomers and polymerization modulators were prepared by emulsion polymerization: TCDHEPT (TEGDMA and DHEPT), BTCDHEPT (Bis-GMA, TEGDMA, and DHEPT), and BTCBPO (Bis-GMA, TEGDMA, and BPO). The capsules were analyzed through Fourier transform infrared spectroscopy and scanning electron microscopy. The capsules were added into experimental photopolymerizable resin composites establishing the following groups: ER (Control without capsules), ER+BPO, ER+BPO+TCDHEPT, and ER+BTCBPO+BTCDHEPT. Filtek Z350 resin composite (3 M ESPE) was used as a commercial reference. The materials were tested for degree of conversion (DC), flexural strength (σf), elastic modulus (Ef), fracture toughness (virgin KIC), self-healing efficiency (healed KIC), and roughness. For statistical analysis, the significance value was established at an a = 0.05 level. RESULTS: When compared to the control material, the incorporation of repairing capsules did not affect DC, σf, and Ef. Fracture toughness was statistically similar between the experimental groups (p ≤ 0.05). Healed KIC was statistically different between the groups ER+TCDHEP and ER+BTCBPO+BTCDHEPT; the self-healing efficiency was higher for ER+TCDHEPT. Surface roughness was statistically similar among all groups. CONCLUSIONS: The use of self-healing capsules promoted repair of the material. Studies with material aging after the self-healing process are necessary to better demonstrate the effectiveness of this system. CLINICAL SIGNIFICANCE: The self-healing system seemed to be a promising technology to be used in self-repaired restorative materials, which may prevent restoration fractures.

Enhanced mechanical properties, anti-biofilm activity, and cytocompatibility of a methacrylate-based polymer loaded with native multiwalled carbon nanotubes.

OBJECTIVES: We aimed to optimize the mechanical and biological properties of a conventional methacrylate-based dental polymer by loading it with double- and triple-walled carbon nanotubes as growth (DTWCNTG). METHODS: A formulation of bisphenol A-glycidyl methacrylate and triethylene glycol dimethacrylate (mass ratio = 2:1) was mixed with DTWCNTG at concentrations of 0.0% (control), 0.001%, 0.005%, and 0.010%. The concentrations were physicochemical and morphologically evaluated, and antibacterial activity was assessed by seeding a Streptococcus mutans strain (ATCC 25175) on the experimental polymeric surfaces. Cellular survival and osteodifferentiation were evaluated in epithelial (HaCat) and preosteoblast cells (MC3T3-E1). RESULTS: The 0.001% DTWCNTG concentration yielded higher compressive strength, elastic modulus, flexural strength, flexural modulus, water sorption, and solubility than the control. The degree of conversion and color did not significantly change with a low amount of DTWCNTG incorporated into the polymer. Antibacterial activity significantly improved when tested on the 0.001% DTWCNTG discs. No groups showed cytotoxicity in a short-term analysis and adding DTWCNTG favored MC3T3-E1 mineralization over the control, particularly in the 0.001% formulation. SIGNIFICANCE: The micro-addition of 0.001% DTWCNTG confers mechanical resistance, antimicrobial properties, and bioactivity to methacrylate-based polymers without significantly compromising color. Incorporating DTWCNTG improved dental composite properties and could be a biomodified material for minimally invasive procedures.

Photopolymerizable dental composite resins with lower shrinkage stress and improved hydrolytic and hygroscopic behavior with a urethane monomer used as an additive.

This work reports the synthesis of a monomer 2-((2-(3-(prop-1-en-2-yl)phenyl)propan-2-yl)carbamoyl)oxy)ethyl methacrylate (MVTPM) and the evaluation of its performance as an additive in the formulation of Bis-GMA/TEGDMA based composite resins. Experimental composite resins formulated with the MVTPM monomer were compared with a control reference. Double bond conversion, polymerization kinetics, shrinkage and associated stress, sorption, and aqueous solubility, cell viability, as well as mechanical properties were evaluated according to international measurements standards. The experimental composite resins show comparable mechanical properties with the control reference and improvements in other properties, such as better hydrolytic and hygroscopic behavior and lower shrinkage stress, are reported. This makes MVTPM monomer potentially useful in the formulation of dental composite resins.

α-amyrin-loaded nanocapsules produce selective cytotoxic activity in leukemic cells.

INTRODUCTION: Amyrins are triterpenes that have attractive pharmacological potential; however, their low water solubility and erratic stomach absorption hinders their use as a drug. The aim of this paper was to develop a novel α-amyrin-loaded nanocapsule for intestinal delivery and evaluate, preliminarily, its cytotoxic ability against leukemic cells. MATERIAL AND METHODS: Five nanocapsule formulations were designed by the solvent displacement-evaporation method. Poly-ε-caprolactone, Eudragit® E100, and Kollicoat® Mae 100 P were used as film-former materials. Particle size, polydispersity index (PdI), zeta potential, and the pH of all formulations were measured. The cytotoxic potential of the nanocapsules was evaluated in vitro using different leukemic lineages RESULTS: Nanocapsules coated with Kollicoat® Mae 100 P presented the smallest particle size (130 nm), the lowest zeta-potential (-38 mV), and the narrowest size distribution (PdI = 0.100). The entrapment efficiency was 65.47%, while the loading capacity was 2.40%. Nanocapsules release 100% of α-amyrin in 40 min (pH 7.4), by using a possible mechanism of swelling-diffusion. The formulation showed excellent on-shelf physicochemical stability during one year. Additionally, nanocapsules produced a selective cytotoxic effect on a human leukemia lineage Kasumi-1, an acute myeloid leukemia cell line, and produced cell death by apoptosis CONCLUSION: α-amyrin-loaded nanocapsules appear to be a promising nanoformulation that could be used against leukemia.

Impact of Drug-Polymer Interaction in Amorphous Solid Dispersion Aiming for the Supersaturation of Poorly Soluble Drug in Biorelevant Medium.

The aim of this study was to investigate the influence of the production method and the polymeric carrier on the ability to generate and maintain the supersaturation of a poorly soluble drug in biorelevant medium. The amorphous solid dispersion of sulfamethoxazole, an antibacterial drug, was produced using two different polymers by spray-drying or hot melt extrusion methods. When Eudragit EPO was used, supersaturation was maintained up to 24 h for both techniques at all drug-polymer proportions. However, when Soluplus was employed in hot melt extrusion, a smaller amount of drug was dissolved when compared to the amorphous drug. The proportion of 3:7 drug-Eudragit EPO (w/w) produced by spray-drying presented a higher amount of drug dissolved in supersaturation studies and it was able to maintain the physical stability under different storage conditions throughout the 90-day evaluation. Supersaturation generation and system stability were found to be related to more effective chemical interaction between the polymer and the drug provided by the production method, as revealed by the 1D ROESY NMR experiment. Investigation of drug-polymer interaction is critical in supersaturating drug delivery systems to avoid crystallization of the drug and to predict the effectiveness of the system. Chemical compounds studied in this article: Sulfamethoxazole (PubChem CID: 4539) and Methacrylate copolymer - Eudragit EPO (PubChem CID: 65358).