Glass ionomer cement particles pre-reacted with chlorhexidine: Physical/chemical properties and antimicrobial activity.

OBJECTIVE: Analyze the effects of the functionalization of pre-functionalized GIC particles with chlorhexidine on the physicochemical properties and antimicrobial activity. MATERIALS AND METHODS: Four groups were prepared: (1) GIC (Bioglass R - Biodinamica) - control group; (2) GIC-CHX 1%: Group containing 1% pre-reacted CHX particles; (3) GIC-CHX 2.5%: Group containing 2.5% pre-reacted CHX particles; (4) GIC-CHX 5%: Group containing 5% pre-reacted CHX particles. Hourglass-shaped specimens (10 mm × 2 mm x 1 mm) were fabricated for mechanical tests including cohesive strength (n = 12), modulus of elasticity (n = 12) and microhardness (n = 10). Discs (10 mm × 2 mm) were prepared for the analysis of Ca+2, PO4- and F- ions release (n = 3), and roughness (n = 12). To evaluate the setting time, a Gilmore needle was used according to ISO 9917-1:2016. Disk-shaped specimens (5 × 1mm) were manufactured and subjected to bacterial activity (n = 9) (Streptococcus mutans ATCC 159). RESULTS: Modulus, roughness, setting time and ions release (Ca+2, PO4-, and F-) there were no statistically significant differences among the groups (p > 0.05). The setting time did not change with the incorporation of CHX. The GIC-CHX 2.5% and GIC-CHX 5% groups exhibited superior antibacterial activity compared to the control group and GIC-CHX 1% (p < 0.001). The GIC-CHX 5% group showed the highest microhardness values (p < 0.041), cohesive strength (p < 0.009) when compared to the control group. CONCLUSION: The pre-reacted CHX in GICs was able to confer antimicrobial activity, improve cohesive strength, microhardness, and did not impair ion release, setting time, and roughness.

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.

Environmental factors modify silver nanoparticles ecotoxicity in Chydorus eurynotus (Cladocera).

Silver nanoparticles (AgNPs) are among the most produced nanomaterials in the world and are incorporated into several products due to their biocide and physicochemical properties. Since freshwater bodies are AgNPs main final sink, several consequences for biota are expected to occur. With the hypothesis that AgNPs can interact with environmental factors, we analyzed their ecotoxicity in combination with humic acids and algae. In addition to the specific AgNPs behavior in the media, we analyzed the mortality, growth, and phototactic behavior of Chydorus eurynotus (Cladocera) as response variables. While algae promoted Ag+ release, humic acids reduced it by adsorption, and their combination resulted in an intermediated Ag+ release. AgNPs affected C. eurynotus survival and growth, but algae and humic acids reduced AgNPs lethality, especially when combined. The humic acids mitigated AgNP effects in C. eurynotus growth, and both factors improved its phototactic behavior. It is essential to deepen the study of the isolated and combined influences of environmental factors on the ecotoxicity of nanoparticles to achieve accurate predictions under realistic exposure scenarios.

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.

Composite Containing Calcium Phosphate Particles Functionalized with 10-MDP.

The phosphate ester monomer 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP) is capable of bonding to hydroxyapatite and, for this reason, is a key component of several self-etch adhesives. In this study, dicalcium phosphate dihydrate particles (DCPD; CaHPO4.2H2O) were functionalized with 10-MDP and used to formulate an experimental composite with 50 vol% inorganic content (3:1 DCPD:silanated barium glass ratio) dispersed in a BisGMA/TEGDMA matrix. The tested hypothesis was that DCPD functionalization would improve the composite's mechanical performance without compromising Ca2+ release. Composites containing nonfunctionalized DCPD or only reinforcing glass (in both cases, with or without 10-MDP mixed in the resin phase) were used as controls. Materials were tested for degree of conversion (DC; by Fourier transform infrared spectroscopy), water sorption (WS) and solubility (SL; according to ISO 4049), biaxial flexural strength (BFS)/modulus (FM) after 24 h and 5 mo in water, and 28-d Ca2+ release in water (by plasma-coupled optical emission spectroscopy). Data were analyzed using analysis of variance/Tukey test (alpha: 5%). DCPD functionalization did not interfere with DC. The composite containing functionalized DCPD showed significantly lower WS and SL in comparison with the material formulated with nonfunctionalized particles. The presence of 10-MDP (as a functionalizing agent or dispersed in the resin phase) reduced the composite's initial BFS and FM. After 5 mo in water, the composite with functionalized DCPD and both glass-only composites were able to maintain their mechanical properties at levels statistically similar to what was observed after 24 h. Ca2+ release was significantly reduced in both formulations containing 10-MDP. In conclusion, DCPD functionalization with 10-MDP increased the composite's resistance to hydrolytic degradation, improving its mechanical stability after prolonged water storage. However, the impaired water transit at the particle-matrix interface led to a reduction in Ca2+ release.

Glass ionomer cement with calcium-releasing particles: Effect on dentin mineral content and mechanical properties.

OBJECTIVE: to evaluate the effect a glass ionomer cement (GIC) containing hydroxyapatite (HAp) or calcium silicate (CaSi) particles on mineral content and mechanical properties of demineralized dentin. Ion release and compressive strength (CS) of the cements were also evaluated. METHODS: GIC (Fuji 9 Gold Label, GC), GIC+ 5%HAp and GIC+ 5%CaSi (by mass) were evaluated. Ion release was determined by induced coupled plasma optical emission spectroscopy (Ca2+/Sr2+) or ion-specific electrode (F-) (n = 3). A composite (Filtek Z250, 3 M ESPE) was used as control in remineralization tests. Demineralized dentin discs were kept in contact with materials in simulated body fluid (SBF) at 37 °C for eight weeks. Mineral:matrix ratio (MMR) was determined by ATR-FTIR spectroscopy (n = 5). Dentin hardness (H) and elastic modulus (E) were determined by nanoindentation (n = 10). CS was tested after 24 h and 7d in deionized water (n = 12). Data were analyzed by ANOVA/Tukey test (α = 0.05). RESULTS: Ca2+ and Sr2+ release was higher for the modified materials (p < 0.05). Only GIC+ 5%HAp showed higher F- release than the control (p < 0.05). All groups showed statistically significant increases in MMR, with no differences among them after 8 weeks (p > 0.05). No differences in dentin H or E were observed among groups (p > 0.05). HAp-modified GIC showed increased initial CS, while adding CaSi had the opposite effect (p < 0.05). After 7 days, GIC+ 5%CaSi presented lower CS in relation to control and GIC+ 5%HAp (p < 0.05). SIGNIFICANCE: GIC modification with HAp or CaSi affected CS and increased ion release; however, none of the groups showed evidence of dentin remineralization in comparison to the negative control.

Antibacterial Activity of a Bioactive Tooth-Coating Material Containing Surface Pre-Reacted Glass in a Complex Multispecies Subgingival Biofilm.

Bioactive materials were developed with the ability to release fluoride and provide some antimicrobial potential, to be widely used in dentistry today. However, few scientific studies have evaluated the antimicrobial activity of bioactive surface pre-reacted glass (S-PRG) coatings (PRG Barrier Coat, Shofu, Kyoto, Japan) on periodontopathogenic biofilms. This study evaluated the antibacterial activity of S-PRG fillers on the microbial profile of multispecies subgingival biofilms. A Calgary Biofilm Device (CBD) was used to grow a 33-species biofilm related to periodontitis for 7 days. The S-PRG coating was applied on CBD pins from the test group and photo-activated (PRG Barrier Coat, Shofu), while the control group received no coating. Seven days after treatment, the total bacterial counts, metabolic activity, and microbial profile of the biofilms were observed using a colorimetric assay and DNA-DNA hybridization. Statistical analyses were applied; namely, the Mann-Whitney, Kruskal-Wallis, and Dunn's post hoc tests. The bacterial activity of the test group was reduced by 25.7% compared with that of the control group. A statistically significant reduction was observed for the counts of 15 species: A. naeslundii, A. odontolyticus, V. parvula, C. ochracea, C. sputigena, E. corrodens, C. gracilis, F. nucleatum polymorphum, F. nucleatum vincentii, F. periodonticum, P. intermedia, P. gingivalis, G. morbillorum, S. anginosus, and S. noxia (p ≤ 0.05). The bioactive coating containing S-PRG modified the composition of the subgingival biofilm in vitro, thereby decreasing colonization by pathogens.

Effect of Biosilicate® Addition on Physical-Mechanical and Biological Properties of Dental Glass Ionomer Cements.

This study investigated the influence of incorporating Biosilicate® on the physico-mechanical and biological properties of glass ionomer cement (GIC). This bioactive glass ceramic (23.75% Na2O, 23.75% CaO, 48.5% SiO2, and 4% P2O5) was incorporated by weight (5%, 10%, or 15%) into commercially available GICs (Maxxion R and Fuji IX GP). Surface characterization was made by SEM (n = 3), EDS (n = 3), and FTIR (n = 1). The setting and working (S/W time) times (n = 3) and compressive strength (CS) were analyzed (n = 10) according to ISO 9917-1:2007. The ion release (n = 6) was determined and quantified by ICP OES and by UV-Vis for Ca, Na, Al, Si, P, and F. To verify cell cytotoxicity, stem cells from the apical papilla (SCAP) were exposed to eluates (n = 3, at a ratio of 1.8 cm2/mL) and analyzed 24 h post-exposure. Antimicrobial activity against Streptococcus mutans (ATCC 25175, NCTC 10449) was analyzed by direct contact for 2 h (n = 5). The data were submitted for normality and lognormality testing. One-way ANOVA and Tukey's test were applied for the working and setting time, compressive strength, and ion release data. Data from cytotoxicity and antimicrobial activity were submitted for Kruskal-Wallis' testing and Dunn's post hoc test (α = 0.05). Among all experimental groups, only those with 5% (wt) of Biosilicate® showed better surface quality. Only M5% showed a comparable W/S time to the original material (p = 0.7254 and p = 0.5912). CS was maintained for all Maxxion R groups (p > 0.0001) and declined for Fuji IX experimental groups (p < 0.0001). The Na, Si, P, and F ions released were significantly increased for all Maxxion R and Fuji IX groups (p < 0.0001). Cytotoxicity was increased only for Maxxion R with 5% and 10% of Biosilicate®. A higher inhibition of S. mutans growth was observed for Maxxion R with 5% of Biosilicate® (less than 100 CFU/mL), followed by Maxxion R with 10% of Biosilicate® (p = 0.0053) and Maxxion R without the glass ceramic (p = 0.0093). Maxxion R and Fuji IX presented different behaviors regarding Biosilicate® incorporation. The impacts on physico-mechanical and biological properties were different depending on the GIC, but therapeutic ion release was increased for both materials.

Resin-modified glass ionomer enriched with BIOGLASS: Ion-release, bioactivity and antibacterial effect.

Developing dental materials for the prevention of remineralization or demineralization is important for high-risk caries patients. This study aimed to evaluate the physicochemical and microbiological effects of adding 45S5 bioglass to resin-modified glass ionomer cement (RMGIC). Samples belonged to the following groups: GIC: conventional glass ionomer cement (Vitro Fil), RMGIC: resin-modified GIC (Vitro Fil LC), and RMGIC/45S5: RMGIC with 10% (wt %) of 45S5. Changes in pH and release of fluoride, calcium, and phosphorus ions under acidic (pH 4) and neutral (pH 7) pH conditions were evaluated. Antibacterial activity was verified based on colony-forming units. Material sorption and solubility were analyzed after bacterial exposure. After 28 days, the bioactivity of the materials was evaluated using scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS). Analysis of variance, post hoc Scheffe, and Tukey (α = 0.05) tests were employed for statistical analysis. RMGIC/45S5 showed higher alkalization activity, calcium release at pH 4 and 7, and sorption than GIC and RMGIC (p < .05). Release of phosphorus and fluoride at pH 4 and 7 was higher for GIC than that for RMGIC and RMGIC/45S5 (p < .05). RMGIC/45S5 showed higher values than RMGIC (p < .05). However, antibacterial activity did not differ among the groups. Precipitates of calcium and phosphorus were visualized in RMGIC/45S5 samples via SEM/EDS. These results indicate that the RMGIC/45S5 promotes alkalization and increases the release of calcium, phosphorus, and fluoride ions, resulting in precipitate deposition rich in calcium and phosphorus, thereby being a promising option to improve the bioactivity of RMGIC.

Ion release and surface roughness of silver soldered bands with two different polishing methods: An in-vitro study.

OBJECTIVE: To evaluate the surface roughness and ion release of silver-soldered joints by using two polishing methods. METHODS: 174 orthodontic bands with and without silver-soldered joints were evaluated and divided into three groups: two experimental, with different polishing methods (SP1 and SP2), and one control (SS) composed of bands without silver solder. For ionic release, 50 bands of each group were immersed in saline solution and submitted to atomic absorption spectrophotometry to quantify the amount of Fe, Ni, Cr (in all the three groups), Ag, Cu, Cd, and Zn (in the two experimental groups). A rugosimeter was employed to verify the surface roughness. RESULTS: Ni and Cr were released in higher amounts after soldering. Cd, Ag, Zn, and Cu may be released from silver-soldered bands independently of the polishing method employed. Ag was released in higher amounts from the soldered bands that presented higher surface roughness. CONCLUSIONS: Differences exist in relation to the surface roughness of silver-soldered bands when distinct polishing methods are used. Toxic ions may be released from silver soldered joints and higher surface roughness may cause higher ionic release.

A Tribological and Ion Released Research of Ti-Materials for Medical Devices.

The increase in longevity worldwide has intensified the use of different types of prostheses for the human body, such as those used in dental work as well as in hip and knee replacements. Currently, Ti-6Al-4V is widely used as a joint implant due to its good mechanical properties and durability. However, studies have revealed that this alloy can release metal ions or particles harmful to human health. The mechanisms are not well understood yet and may involve wear and/or corrosion. Therefore, in this work, commercial pure titanium and a Ti-6Al-4V alloy were investigated before and after being exposed to a simulated biological fluid through tribological tests, surface analysis, and ionic dissolution characterization by ICP-AES. Before exposure, X-ray diffraction and optical microscopy revealed equiaxed α-Ti in both materials and ß-Ti in Ti-6Al-4V. Scratch tests exhibited a lower coefficient of friction for Ti-6Al-4V alloy than commercially pure titanium. After exposure, X-ray photoelectron spectroscopy and surface-enhanced Raman spectroscopy results showed an oxide film formed by TiO2, both in commercially pure titanium and in Ti-6Al-4V, and by TiO and Al2O3 associated with the presence of the alloys. Furthermore, inductively coupled plasma atomic emission spectroscopy revealed that aluminum was the main ion released for Ti-6Al-4V, giving negligible values for the other metal ions.

Mechanical and Antimicrobial Polyethylene Composites with CaO Nanoparticles.

Low-density polyethylene composites containing different sizes of calcium oxide (CaO) nanoparticles were obtained by melt mixing. The CaO nanoparticles were synthesized by either the sol-gel or sonication methods, obtaining two different sizes: ca. 55 nm and 25 nm. These nanoparticles were used either as-synthesized or were modified organically on the surface with oleic acid (Mod-CaO), at concentrations of 3, 5, and 10 wt% in the polymer. The Mod-CaO nanoparticles of 25 nm can act as nucleating agents, increasing the polymer's crystallinity. The Young's Modulus increased with the Mod-CaO nanoparticles, rendering higher reinforcement effects with an increase as high as 36%. The reduction in Escherichia coli bacteria in the nanocomposites increased with the amount of CaO nanoparticles, the size reduction, and the surface modification. The highest antimicrobial behavior was found in the composites with a Mod-CaO of 25 nm, presenting a reduction of 99.99%. This strong antimicrobial effect can be associated with the release of the Ca2+ from the composites, as studied for the composite with 10 wt% nanoparticles. The ion release was dependent on the size of the nanoparticles and their surface modification. These findings show that CaO nanoparticles are an excellent alternative as an antimicrobial filler in polymer nanocomposites to be applied for food packaging or medical devices.

Development of brushite particles synthesized in the presence of acidic monomers for dental applications.

OBJECTIVES: To synthesize and characterize brushite particles in the presence of acidic monomers (acrylic acid/AA, citric acid/CA, and methacryloyloxyethyl phosphate/MOEP) and evaluate the effect of these particles on degree of conversion (DC), flexural strength/modulus (FS/FM) and ion release of experimental composites. METHODS: Particles were synthesized by co-precipitation with monomers added to the phosphate precursor solution and characterized for monomer content, size and morphology. Composites containing 20 vol% brushite and 40 vol% reinforcing glass were tested for DC, FS and FM (after 24 h and 60 d in water), and 60-day ion release. Data were subjected to ANOVA/Tukey tests (DC) or Kruskal-Wallis/Dunn tests (FS and FM, alpha: 5%). RESULTS: The presence of acidic monomers affected particle morphology. Monomer content on the particles was low (0.1-1.4% by mass). Composites presented similar DC. For FS/24 h, only the composite containing DCPD_AA was statistically similar to the composite containing 60 vol% of reinforcing glass (without brushite, "control"). After 60 days, all brushite-containing materials showed similar FS, statistically lower than the control composite (p<0.01). Composites containing DCPD_AA, DCPD_MOEP or DCPD_U ("unmodified") showed statistically similar FM/24 h, higher than the control composite. After prolonged immersion, all composites were similar to the control composite, except DCPD_AA. Cumulative ion release ranged from 21 ppm to 28 ppm (calcium) and 9 ppm to 17 ppm (phosphate). Statistically significant reductions in ion release between 15 and 60 days were detected only for the composite containing DCPD_MOEP. SIGNIFICANCE: Acidic monomers added to the synthesis affected brushite particle morphology. After 60-day storage in water, composite strength was similar among all brushite-containing composites. Ion release was sustained for 60 days and it was not affected by particle morphology.

Effect of Alkaline Peroxides on the Surface of Cobalt Chrome Alloy: An In Vitro Study.

PURPOSE: Removable denture hygiene care is very important for the longevity of the rehabilitation treatment; however, it is necessary to analyze the effects that denture cleansers can cause on the surfaces of prostheses. Thus, this study evaluated the effect of alkaline peroxide-effervescent tablets on the surface of cobalt-chromium alloys (Co-Cr) used in removable partial dentures. MATERIALS AND METHODS: Circular metallic specimens (12 × 3 mm) were fabricated and were immersed (n = 16) in: control, Polident 3 Minute (P3M), Steradent (S), Efferdent (E), Polident for Partials (PFP), and Corega Tabs (CT). The surface roughness (µm) (n = 10) was measured before and after periods of cleanser immersion corresponding to 0.5, 1, 2, 3, 4, and 5 years. Ion release was analyzed (n = 5) for Co, Cr, and molybdenum (Mo). Scanning electron microscopy (SEM) analysis and an Energy-dispersive X-ray spectroscopy (EDS) were conducted in one specimen. The surface roughness data were statistically analyzed (α = 0.05) with the Kruskal-Wallis test to compare the solutions, and the Friedman test compared the immersion durations. Ion release analysis was performed using 2-way ANOVA and Tukey's test. RESULTS: There was no significant surface roughness difference when comparing the solutions (p > 0.05) and the immersion durations (p = 0.137). Regarding ion release (µg/L), CT, E, and control produced a greater release of Co ions than S (p < 0.05). CT produced a greater release of Cr ions than control, S, and P3M (p < 0.05). Finally, E caused the greatest release of Mo ions (p < 0.05). SEM confirmed that the solutions did not damage the surfaces and EDS confirmed that there were no signs of oxidation. CONCLUSION: The various solutions tested did not have any deleterious effects on the Co-Cr alloy surface. Steradent, however, presented the smallest ionic release.

Synthesis of silver-containing calcium aluminate particles and their effects on a MTA-based endodontic sealer.

OBJECTIVE: To synthetize calcium aluminate (C3A) and silver-containing C3A particles (C3A+Ag) testing their effects on the properties of a MTA-based endodontic sealer in comparison to an epoxy resin- and a calcium silicate-based sealer. METHODS: Pure C3A and C3A+Ag particles were synthesized by a chemical method and characterized using XRD to identify crystalline phases. SEM/EDS analysis investigated morphology, particle size, and elemental composition of particles. Setting time, flow, radiopacity, water sorption and solubility of commercial and modified sealers were evaluated according to ISO 6876/2012. The pH and ions release were measured using a pHmeter and a microwave induced plasma optical emission spectrometer. The inhibition of biofilm growth was evaluated by confocal laser scanning microscopy (CLSM). Data were rank transformed and analyzed by ANOVA and Tukey test (P<0.05). RESULTS: The C3A particles showed an irregular grain agglomerated structure with voids and pores. In C3A+Ag particles, Ag modified the material morphology, confirming the deposition of Ag. The physicochemical properties of the modified MTA-based sealer were similar to the commercial material, except for the significant increase in Ca+2 release. However, there was no Ag release. Setting time, flow, radiopacity, water sorption and solubility were adequate for all materials. All the materials showed alkaline pH. Antibiofilm effect was improved in the presence of C3A particles, while the biofilm inhibition was lower in the presence of Ag. SIGNIFICANCE: The modified sealer presented improved antibiofilm properties and calcium release, without dramatic effects on the other characteristics. It is expected a positive effect in its antimicrobial behavior.

Ion-releasing dental restorative composites containing functionalized brushite nanoparticles for improved mechanical strength.

OBJECTIVES: This study describes the synthesis of brushite nanoparticles (CaHPO4·2H2O) 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.

Synthesis and characterization of silver phosphate/calcium phosphate mixed particles capable of silver nanoparticle formation by photoreduction.

Silver phosphate is a semi-conductor sensitive to UV-Vis radiation (<530nm). Exposure to radiation removes electrons from the oxygen valence shell, which are scavenged by silver cations (Ag+), forming metallic silver (Ag0) nanoparticles. The possibility of silver nanoparticle formation in situ by a photoreduction process was the basis for the application of mixed calcium phosphate/silver phosphate particles as remineralizing and antibacterial fillers in resin-based dental materials. Mixed phosphate particles were synthesized, characterized and added to a dimethacrylate resin in 20% or 30% mass fractions to investigate their efficacy as ion-releasing fillers for dental remineralization and antibacterial activity. The formation of metallic silver nanoparticles after exposure to visible radiation from a dental curing unit (peak emission: 470nm) was demonstrated by particle X-ray diffraction and scanning electron microscopy analysis of the composite fractured surface. Calcium and phosphate release from materials containing the mixed particles were similar to those containing pure CaP particles, whereas Streptococcus mutans colonies were reduced by three orders of magnitude in relation to the control, which can be attributed to silver release. As expected, the optical properties of the materials containing mixed phosphate particles were compromised by the presence of silver. Nevertheless, materials containing mixed phosphate particles presented higher fracture strength and elastic modulus than those with pure CaP particles.

Polymer-based material containing calcium phosphate particles functionalized with a dimethacrylate monomer for use in restorative dentistry.

Dicalcium phosphate dihydrate particles functionalized with triethyleneglycol dimethacrylate were synthesized and added to a photocurable mixture of bisphenol-A glycidyl dimethacrylate and triethyleneglycol dimethacrylate with the purpose of developing a resin composite capable of releasing calcium and phosphate ions to foster dental remineralization. Particle functionalization would minimize the deleterious effect of adding low cohesive strength nano-structured particles with no chemical interaction with the organic matrix on the material's mechanical properties. The results showed that calcium release over 28 days was not impaired by particle functionalization. A statistically significant 32% increase in strength was recorded with the use of functionalized dicalcium phosphate dihydrate in comparison to the material containing non-functionalized particles. However, the strength of the unfilled resin was not matched by the composite with functionalized particles. Elastic modulus increased with particle incorporation, regardless of functionalization. Degree of conversion and optical properties (total transmittance and color change/ΔE) of the resin-based materials were not affected by the addition of dicalcium phosphate dihydrate particles (functionalized or not).

Avaliação do pH, liberação de íons cálcio e atividade antimicrobiana do cimento Portland associado a Bambusa textilis em diferentes proporções / Analysis of pH, calcium ion release and antibacterial activity of Portland cement associated to Bambusa textilis in different proportion

Introdução: há uma busca incessante por agentes fitoterápicos na medicina e odontologia. Dentro da endodontia, busca-se uma substância que potencialize os efeitos biológicos e antimicrobianos do hidróxido de cálcio como curativo de demora. Não há na literatura relatos sobre a associação do cimento Portland com a Bambusa textilis, uma planta nativa da China, onde é usada na elaboração de medicamentos, pois se trata de uma fonte importante de resinas, sendo, portanto utilizadas por seu poder anti-inflamatório, anticatarral, anticonvulsivante e antitérmico. Sabendo da semelhança do cimento Portland com o MTA, e que esse ultimo apresenta bons resultados físico-químicos, surge a dúvida da possibilidade da associação, com a finalidade de melhorar as atividades antimicrobianas, e a interferência na liberação de íons cálcio e hidroxila. Objetivo: avaliar o pH, liberação de íons cálcio e atividade antimicrobiana do cimento Portland associado a Bambusa textilis em diferentes proporções. Metodologia: os cimentos experimentais foram 3 g Cimento Portland + 1,2 ml de Bambusa textilis (G1); 3 g Cimento Portland + 0,6 ml de água + 0,6 de Bambusa textilis (G2); 3 g Cimento Portland + 0,9 ml água + 0,3 ml de Bambusa textilis (G3); 3 g Cimento Portland puro (controle) + 1,2 ml água (G4); Bambusa textilis (controle): 20 microlitros por poço. Para os testes de pH e liberação de íons cálcio foram utilizados tubos de polietileno, os quais foram preenchidos com os cimentos e imersos em frascos contendo água deionizada. As mensurações foram por meio de um peagâmetro e espectrofotômetro de absorção atômica. Para a análise da atividade antimicrobiana, foi utilizada a técnica de difusão radial com cepa de Enterococcus faecalis. Os halos de inibição foram mensurados com auxílio de um paquímetro digital. A análise estatística foi realizada pelo teste ANOVA para comparação global, e teste de Tukey para comparações individuais, com significância de 5%. Resultados: os valores de pH se mostraram próximos ao neutro para todos os grupos em todos os períodos experimentais. Houve liberação de íons cálcio e ocorreu em todos os grupos e em todos os períodos experimentais. Em relação à atividade antimicrobiana, nenhuma das proporções apresentou atividade. Conclusão: a associação da Bambusa textilis ao cimento Portland manteve seu pH e liberação de íons cálcio, mas não potencializou sua atividade antimicrobiana frente ao E. faecalis. (AU)

Introduction: there is a search for phytotherapeutic agents in medicine and dentistry. Within endodontics, a substance that potentiates the biological and antimicrobial effects of calcium hydroxide as a delay dressing is sought. There are no reports in the literature about the association of Portland cement with Bambusa textilis, a plant native to China, where it is used in the manufacture of medicines, since it is an important source of resins and is therefore used for its anti-inflammatory power, anticonvulsive and antipyretic. Knowing the similarity of the Portland cement with the MTA, and that the latter presents good physicochemical results, the possibility of the association arises, with the purpose of improving the antimicrobial activities, and the interference in the release of calcium and hydroxyl ions. Aim: to analyze the pH, calcium ion release and antibacterial activity of Portland cement associated to Bambusa textilis in different proportions. Methods: the experimental cements ́ proportions were: 3 g of Portland cement + 1.2 ml of Bambusa textilis (G1); 3 g of Portland cement + 0.6 ml of water + 0.6 of Bambusa textilis (G2); 3 g of Portland cement + 0.9 ml of water + 0.3 ml of Bambusa textilis (G3); 3 g of pure Portland cement (control group) + 1.2 ml of water (G4); Bambusa textilis (control group): 20 µLper well. Polyethylene tubes filled with the cements and immersed in deionized water were employed. Calcium ion release was analyzed using an atomic absorption spectrophotometer and the change in pH was determined through a pH meter. For the analysis of antibacterial activity, a digital radial diffusion assay with a Enterococcus faecalis strain was utilized. Statistical analysis was performed using ANOVA and Tukey's tests. The level of significance was set at P = 0.05. Results: pH values were close to neutral for all of the experimental groups in all periods evaluated. Calcium ion release was observed in all experimental groups and evaluation periods. Regarding the antibacterial activity, this property could not be detected in any of the proportions used in this study. Conclusions: the association of Bambusa textilis to Portland cement, preserved its pH values and its calcium ion release property. Nevertheless, it did not improve its antibacterial activity against E. faecalis strains. (AU)

Bioactive composites containing TEGDMA-functionalized calcium phosphate particles: Degree of conversion, fracture strength and ion release evaluation.

OBJECTIVE: To evaluate the strength and ion release of experimental composites containing TEGDMA-functionalized calcium phosphate particles. METHODS: Seven composites containing equal parts (in mols) of BisGMA and TEGDMA and 60vol% of fillers were manipulated. Filler phase was constituted by silanized barium glass and 0% (control), 10% or 20% (volume) of dicalcium phosphate dihydrate (DPCD) particles, either non-functionalized or functionalized with two different TEDGMA contents. DCPD particles were synthesized and characterized by X-ray diffraction (XRD), elemental analysis, surface area and dynamic light scattering. Composites were tested for degree of conversion (DC) by near-FTIR. Biaxial flexural strength (BFS) was determined after 24h and 28days in water. Calcium and phosphate release after 7days was assessed using inductively coupled plasma optical emission spectrometry (ICP-OES). Data were analyzed by ANOVA/Tukey test (alpha:5%). RESULTS: XRD confirmed the crystalline structure corresponding to DCPD. Elemental analysis revealed particles with zero, 14% or 22% TEGDMA, with similar D50 (around 19µm) and surface areas from 3.5 to 11.4m2/g. The presence of DCPD did not reduce DC. After 24h, functionalization (both 14% and 22% TEGDMA) improved composite strength in comparison to non-functionalized DCPD, both at 10% and 20% levels. After 28days, BFS of materials containing 10% functionalized DCPD were statistically similar to the control containing only barium glass. Among composites containing 10% DCPD, particle functionalization with 14% TEGDMA did not jeopardize ion release. SIGNIFICANCE: At 10vol%, the use of TEGDMA-functionalized CaP particles improved composite strength in relation to non-functionalized particles, while maintaining similar ion release levels.