Use of Piranha Solution as An Alternative Route to Promote Bioactivation of PEEK Surface with Low Functionalization Times.

This study aimed to achieve bioactivity on the PEEK surface using piranha solution through a lower functionalization time. For this purpose, the functionalization occurred with piranha solution and 98% sulfuric acid in the proportions of 1:2, 1:1, and 2:1 at periods of 30, 60, and 90 s. The samples treated for longer times at higher concentrations registered the characteristic spectroscopy band associated with sulfonation. Additionally, both chemical treatments allowed the opening of the aromatic ring, increasing the number of functional groups available and making the surface more hydrophilic. The piranha solution treatments with higher concentrations and longer times promoted greater heterogeneity in the surface pores, which affected the roughness of untreated PEEK. Furthermore, the treatments induced calcium deposition on the surface during immersion in SBF fluid. In conclusion, the proposed chemical modifications using sulfuric acid SPEEK 90 and, especially, the piranha solution PEEK-PS 2:1-90, were demonstrated to be promising in promoting the rapid bioactivation of PEEK-based implants.

Analysis of Tissue Repair of a New Cement Based on Calcium and Strontium Aluminates: A Triple-Blinded, Randomized, Controlled Trial in an Animal Model.

OBJECTIVE: The focus of this triple-blind randomized study was to evaluate the biocompatibility of a new root canal filling sealer (RCFS) based on tristrontium aluminate and dodecacalcium hepta-aluminate in living tissue. MATERIAL AND METHODS: Forty-five Wistar rats (Rattus norvegicus) were divided into three groups: control (polyethylene), sealer (Bio-C Sealer, Londrina, PR, Brazil), and experimental (tristrontium aluminate and dodecacalcium hepta-aluminate). The tissues were analyzed under an optical microscope to assess different cellular events at different time intervals (7, 15, and 30 days). STATISTICAL ANALYSIS: Data were analyzed using the Kruskal-Wallis and Dunn (p < 0.05) tests. RESULTS: In the initial period, a moderate inflammatory infiltrate was observed, similar between the endodontic cements groups (p = 0.725). The intensity of the infiltrate decreased with time, with no significant difference among the groups (p > 0.05). The number of young fibroblasts was elevated in all groups evaluated at 7 days. The experimental group showed the highest number of cells at all time intervals, but the difference with the sealer group at 7 (p = 0.001) and 15 days (p = 0.002) and the control group at 30 days was not significant (p = 0.001). Regarding tissue repair events, the amount of collagen fibers increased over the experimental intervals, with no significant difference between the sealer and control groups (p > 0.05). CONCLUSION: The experimental RCFS based on calcium and strontium aluminates proved to be biocompatible for use in close contact with periapical tissue, inducing a low inflammatory reaction and favoring rapid tissue repair.

Chitosan/Gelatin Scaffolds Loaded with Jatropha mollissima Extract as Potential Skin Tissue Engineering Materials.

This work aimed to develop chitosan/gelatin scaffolds loaded with ethanolic extract of Jatropha mollissima (EEJM) to evaluate the influence of its content on the properties of these structures. The scaffolds were prepared by freeze-drying, with different EEJM contents (0-10% (w/w)) and crosslinked with genipin (0.5% (w/w)). The EEJM were characterized through High Performance Liquid Chromatography coupled to a Diode Array Detector (HPLC-DAD), and the determination of three secondary metabolites contents was accomplished. The physical, chemical and biological properties of the scaffolds were investigated. From the HPLC-DAD, six main substances were evidenced, and from the quantification of the total concentration, the condensed tannins were the highest (431.68 ± 33.43 mg·g-1). Spectroscopy showed good mixing between the scaffolds' components. Adding and increasing the EEJM content did not significantly influence the properties of swelling and porosity, but did affect the biodegradation and average pore size. The enzymatic biodegradation test showed a maximum weight loss of 42.89 within 28 days and reinforced the efficiency of genipin in crosslinking chitosan-based materials. The addition of the extract promoted the average pore sizes at a range of 138.44-227.67 µm, which is compatible with those reported for skin regeneration. All of the scaffolds proved to be biocompatible for L929 cells, supporting their potential application as skin tissue engineering materials.

Physicochemical, Morphological, and Cytotoxic Properties of Brazilian Jackfruit (Artocarpus heterophyllus) Starch Scaffold Loaded with Silver Nanoparticles.

Due to the physical, thermal, and biological properties of silver nanoparticles (AgNPs), as well as the biocompatibility and environmental safety of the naturally occurring polymeric component, polysaccharide-based composites containing AgNPs are a promising choice for the development of biomaterials. Starch is a low-cost, non-toxic, biocompatible, and tissue-healing natural polymer. The application of starch in various forms and its combination with metallic nanoparticles have contributed to the advancement of biomaterials. Few investigations into jackfruit starch with silver nanoparticle biocomposites exist. This research intends to explore the physicochemical, morphological, and cytotoxic properties of a Brazilian jackfruit starch-based scaffold loaded with AgNPs. The AgNPs were synthesized by chemical reduction and the scaffold was produced by gelatinization. X-ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS), and Fourier-transform infrared spectroscopy (FTIR) were used to study the scaffold. The findings supported the development of stable, monodispersed, and triangular AgNPs. XRD and EDS analyses demonstrated the incorporation of silver nanoparticles. AgNPs could alter the scaffold's crystallinity, roughness, and thermal stability without affecting its chemistry or physics. Triangular anisotropic AgNPs exhibited no toxicity against L929 cells at concentrations ranging from 6.25 × 10-5 to 1 × 10-3 mol·L-1, implying that the scaffolds might have had no adverse effects on the cells. The scaffolds prepared with jackfruit starch showed greater crystallinity and thermal stability, and absence of toxicity after the incorporation of triangular AgNPs. These findings indicate that jackfruit is a promising starch source for developing biomaterials.

A novel N95 respirator with chitosan nanoparticles: mechanical, antiviral, microbiological and cytotoxicity evaluations.

BACKGROUND: It is known that some sectors of hospitals have high bacteria and virus loads that can remain as aerosols in the air and represent a significant health threat for patients and mainly professionals that work in the place daily. Therefore, the need for a respirator able to improve the filtration barrier of N95 masks and even inactivating airborne virus and bacteria becomes apparent. Such a fact motivated the creation of a new N95 respirator which employs chitosan nanoparticles on its intermediate layer (SN95 + CNP). RESULTS: The average chitosan nanoparticle size obtained was 165.20 ± 35.00 nm, with a polydispersity index of 0.36 ± 0.03 and a zeta potential of 47.50 ± 1.70 mV. Mechanical tests demonstrate that the SN95 + CNP respirator is more resistant and meets the safety requisites of aerosol penetration, resistance to breath and flammability, presenting higher potential to filtrate microbial and viral particles when compared to conventional SN95 respirators. Furthermore, biological in vitro tests on bacteria, fungi and mammalian cell lines (HaCat, Vero E6 and CCL-81) corroborate the hypothesis that our SN95 + CNP respirator presents strong antimicrobial activity and is safe for human use. There was a reduction of 96.83% of the alphacoronavirus virus and 99% of H1N1 virus and MHV-3 betacoronavirus after 120 min of contact compared to the conventional respirator (SN95), demonstrating that SN95 + CNP have a relevant potential as personal protection equipment. CONCLUSIONS: Due to chitosan nanotechnology, our novel N95 respirator presents improved mechanical, antimicrobial and antiviral characteristics.

Brushite bone cement containing polyethylene glycol for bone regeneration.

BACKGROUND: Bone cements aid in bone regeneration; however, if the handling time is not well established for the material to harden, complications may arise. OBJECTIVE: This work investigates the effect of using polyethylene glycol (PEG) and characterize it in brushite bone cement in order to obtain desirable handling times as well as its regeneration in vivo to analyse if addition of this polymer may significantly modify its properties. METHODS: PEG 4000 was synthesised with wollastonite by phosphorization reaction in order to form brushite which was further cured by oven drying. They were further characterised and tested in vivo as tibial bone defect model using rabbits. RESULTS: Addition of PEG exhibited handling times of 60 min with a low increase in temperature when curing. Brushite phase of ∼71% was obtained after cement hardening with good compressive strength (25 MPa) and decent values of porosity (33%). In vivo presented that, at 40 days postoperatively, accelerated bone neoformation with partial consolidation at 30 days and total after 60 days when using bone cement. CONCLUSIONS: Addition of PEG does not disrupt the beneficial properties of the bone cement and can be a potential alternative to control the time-temperature profile of hardening these materials.

Surface Bioactivation of Polyether Ether Ketone (PEEK) by Sulfuric Acid and Piranha Solution: Influence of the Modification Route in Capacity for Inducing Cell Growth.

The aim of this study was to promote bioactivity of the PEEK surface using sulfuric acid and piranha solution. PEEK was functionalized by a sulfuric acid treatment for 90 s and by piranha solution for 60 and 90 s. Chemical modification of the PEEK surface was evaluated by infrared spectroscopy, contact angle analysis, cytotoxicity, cell adhesion and proliferation. The spectroscopy characteristic band associated with sulfonation was observed in all treated samples. PEEK with piranha solution 60 s showed an increase in the intensity of the bands, which was even more significant for the longer treatment (90 s). The introduction of the sulfonic acid functional group reduced the contact angle. In cytotoxicity assays, for all treatments, the number of viable cells was higher when compared to those of untreated PEEK. PEEK treated with sulfuric acid and piranha solution for 60 s were the treatments that showed the highest percentage of cell viability with no statistically significant differences between them. The modified surfaces had a greater capacity for inducing cell growth, indicative of effective cell adhesion and proliferation. The proposed chemical modifications are promising for the functionalization of PEEK-based implants, as they were effective in promoting bioactivation of the PEEK surface and in stimulating cell growth and proliferation.

Biocompatible Sulphonated PEEK Spheres: Influence of Processing Conditions on Morphology and Swelling Behavior.

This work aimed to develop and evaluate the influence of processing variables on the morphology and swelling of sulfonated poly(ether ether ketone) (SPEEK) spheres for possible applications as a biomaterial. We used the drip method to obtain spheres with the polymer starting solutions SPEEK-6 (w/v: 6%) and SPEEK-10 (w/v: 10%), drip rates (20 and 30 mL/h), and drip heights (5 and 10 cm) in experimental planning. The samples were characterized by Fourier-transform infrared spectroscopy (FTIR), optical microscopy (OM), the absorption capacity of phosphate-buffered saline (PBS) by swelling (%), and statistical analysis of data through Design of Experiments (DOE). The obtained results evidenced that the processing variables influenced the morphology and swelling. Spheres with a bigger concentration of the polymer solution presented a greater degree of sulfonation (DS). We verified that the diameter of the spheres was directly related to the variable height and the sphericity was associated with the speed and viscosity of the solution. Bigger and more pores in a greater amount were observed in the spheres with a greater DS, influencing the behavior of the swelling in PBS. The better variable combinations with a high DS, regular sphericity, a smaller diameter, and greater swelling were the samples S2-10-20-5 e S10-10-20-5. The cytotoxicity indicated that the best samples obtained in the experimental planning (S2-10-20-5 and S10-10-20-5) were not toxic. In that regard, the evaluated spheres presented cell viability and swelling capacity, suggesting their possible applications as biomaterials.

Development of Gelatin/Misoprostol Compounds for Use in Pregnancy Failures.

Early abortion is one of the most common complications during pregnancy. However, the frequent handling of the genital region, more precisely the vagina, which causes discomfort to patients in this abortion process due to the frequency of drug insertion, as four pills are inserted every six hours, has led to the search for alternatives to alleviate the suffering caused by this practice in patients who are already in a shaken emotional state. Hence, this work aimed to develop composites of gelatin and misoprostol, using a conventional single-dose drug delivery system. These composites were prepared by freeze/lyophilization technique, by dissolving the gelatin in distilled water, with a concentration of 2.5% (w/v), and misoprostol was incorporated into the gelatin solution at the therapeutic concentration (800 mcg). They were subsequently molded, frozen and lyophilized. The samples of the composites were then crosslinked with sodium tripolyphosphate (TPP) 1% (v/v) with respect to the gelatin mass for 5 min. The characterization techniques used were: Optical Microscopy (OM), Fourier Transformed Infrared Spectroscopy (FTIR), Thermogravimetry (TG), Swelling, Biodegradation and Cytotoxicity. In OM it was observed that the addition of the drug improved the cylindrical appearance of the compounds, in comparison with the sample that was composed of only gelatin. There was a reduction in the degree of swelling with the addition of the drug and crosslinking. The cytotoxicity test indicated the biocompatibility of the material. Based on the results obtained in these tests, the composites have therapeutic potential for uterine emptying in pregnancy failures, especially in the first trimester.

Chitosan-Based Biomaterial, Calcium Hydroxide and Chlorhexidine for Potential Use as Intracanal Medication.

The objective of this study was to develop a chitosan-based biomaterial with calcium hydroxide and 2% chlorhexidine for intracanal treatment application and, consequently, to diminish the number of microorganisms in the root canal system. The chitosan solution was prepared by dissolving it in 2% and 4% acetic acid (v/v) for 1 h at room temperature (25 °C) with magnetic agitation (430 rpm). Calcium hydroxide was obtained in two stages: the first was the synthesis of the calcium oxide-CaO, and the second was that of the calcium hydroxide-Ca(OH)2. The samples were developed using different concentrations of chitosan, calcium hydroxide, and chlorhexidine 2%. They were codified as Ca(OH)2 + Q2% (M1), Ca(OH)2 + Q4% (M2), Ca(OH)2 + Q2% + CLX (M3), Ca(OH)2 + Q4% + CLX (M4), Ca(OH)2 + Q2% + PEG (M5), and Ca(OH)2 + Q4% + PEG (M6). They were characterized through Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and rheological measurement, and the antimicrobial activity was evaluated in vitro. Characteristic absorption bands of the source materials used in this research were observed in the FTIR spectra. The X-ray diffraction technique indicated that the material has a semi-crystalline structure and that the presence of calcium hydroxide made the biomaterial more crystalline. The viscosity measurement showed a pseudoplastic behavior of the studied samples. The microbiologic analysis was positive for all samples tested, with bigger inhibition zones for the samples M3 and M4. As a result, we conclude that the formulation developed based on chitosan is promising and has potential to be an intracanal medication.

In vivo Hemostatic Activity of Jatropha mollissima: A Triple-Blinded, Randomized, Controlled Trial in an Animal Model.

OBJECTIVE: The objective of this study was to evaluate the hemostatic activity of the sap from Jatropha mollissima (Pohl) Baill. in rats. MATERIALS AND METHODS: Twenty-four Wistar rats were randomized into four groups (n = 6): the JM25 and JM40 groups were treated with ethanolic extract from the sap of J. mollissima, in a concentration of 25 and 40 mg·mL1, respectively; the MO group was treated with Monsel's solution and the control group SC with a 0.9% sodium chloride solution. STATISTICAL ANALYSIS: Data were submitted to the Kurskal-Wallis' test, followed by Dunn's post hoc (p < 0.05). RESULTS: There was a significant reduction in the bleeding time of the group from the JM25 extract (p = 0.001) when compared with MO and SC. There were no statistically significant differences between groups JM25 and JM40 (p > 0.05). The JM25 group did not present rebleeding, a result significantly different from the MO group (p = 0.001). Monsel's solution showed significant bleeding, six times greater than the control group SC. CONCLUSION: The J. mollissima extract, in the concentration of 25 mg·mL1, showed the highest hemostatic efficiency and was found to be a promising biomaterial for the elaboration of a hemostatic product.

Injectable bone substitute based on chitosan with polyethylene glycol polymeric solution and biphasic calcium phosphate microspheres.

We described a method to produce an injectable bone substitute consisting of a solid and liquid phase, this solid was formed using the coacervation method consisting of a mixture of Hydroxyapatite (HAp) and beta-Tricalcium Phosphate (ß-TCP) which the sodium alginate - precursor - was removed during sinterization. The biphasic calcium phosphate microspheres had varying size distributions depending on the flow rate and these microspheres were mixed with a polymeric solution, chitosan and polyethylene glycol, and depending on the ratio of these phases, the injectability results varied. Nonetheless, the force required for complete removal will not disrupt the accuracy of injection into the bone defect while the biomaterial exhibited no cytotoxicity with promising results from in vivo using tibia bone defect in rabbits at 30 and 60 days whereas bone repair was more intense and accentuated with the usage of the biomaterial, and was gradually absorbed during the evaluated periods.

Chitosan Woven Meshes: Influence of Threads Configuration on Mechanical, Morphological, and Physiological Properties.

This study aimed to develop meshes from the weaving of mono- and multifilament wet-spun chitosan (CS), for possible biomedical applications. In the wet-spinning process, CS solution (4% w/v) was extruded in a coagulation bath containing 70% sodium hydroxide solution (0.5 M), and 30% methanol was used. The multifilament thread was prepared by twisted of two and three monofilaments. CS threads obtained were characterized by tensile tests and scanning electron microscopy (SEM). Moreover, it was verified from the morphological tests that threads preserve the characteristics of the individual filaments and present typical "skin-core" microstructure obtained by wet spinning. CS woven meshes obtained were evaluated by optical microscopy (OM), tensile test, swelling degree, and in vitro enzymatic biodegradation. Mechanical properties, biodegradation rate, and amount of fluid absorbed of CS woven meshes were influenced by thread configuration. Hydrated CS meshes showed a larger elastic zone than the dry state. Therefore, CS woven meshes were obtained with modular properties from thread configuration used in weaving, suggesting potential applications in the biomedical field, like dressings, controlled drug delivery systems, or mechanical support.

Progress in the Development of Chitosan Based Insulin Delivery Systems: A Systematic Literature Review.

Diabetes mellitus is a chronic disease that is considered a worldwide epidemic, and its control is a constant challenge for health systems. Since insulin had its first successful use, scientists have researched to improve the desired effects and reduce side-effects. Over the years, the challenge has been to increase adherence to treatment and improve the quality of life for diabetics by developing an insulin delivery system. This systematic review (SR) analyses experimental articles from 1998 to 2018 related to the development of the chitosan/insulin delivery system (CIDS). Automated support: Start tool was used to perform part of these activities. The search terms "insulin", "delivery or release system", and "chitosan" were used to retrieve articles in PubMed, Science Direct, Engineering Village, and HubMed. A total of 55 articles were selected. The overview, phase, model, way of administration, and the efficiency of CIDS were analyzed. According to SR results, most of the articles were published from 2010 onwards, representing 72.7% of the selected papers, and research groups from China publicized 23.6% of the selected articles. According to the SR, 51% of the studies were carried out in vivo and 45% in vitro. Most of the systems were nanoparticle based (54.8%), and oral administration was proposed by 60.0% of the selected articles. Only 36.4% performed loaded capacity and encapsulation efficiency assays, and 24 h (16.4%), 12 h (12.7%), and 6 h (11.0%) were the most frequent insulin release times. Chitosan's intrinsic characteristics, which include biodegradability, biocompatibility, adhesiveness, the ability to open epithelial tight junctions to allow an increase in the paracellular transport of macromolecular drugs, such as insulin, and the fact that it does not result in allergic reactions in the human body after implantation, injection, topical application or ingestion, have contributed to the increase in research of CIDS over the years. However, the number of studies is still limited and the use of an alternative form of insulin administration is not yet possible. Thus, more studies in this area, aiming for the development of an insulin delivery system that can promote more adherence to the treatment and patient comfort, are required.

Effect of chitosan and Dysphania ambrosioides on the bone regeneration process: A randomized controlled trial in an animal model.

The focus of this triple-blind study was on evaluating the effect of chitosan combined with Dysphania ambrosioides (A) extract on the bone repair process in vivo. In total, 60 male Wistar rats (Rattus norvegicus albinus) weighing between 260 and 270 g were randomly selected for this study and distributed into four groups (n = 15). Group C (chitosan), Group CA5 (chitosan + 5% of D. ambrosioides), Group CA20 (chitosan + 20% of D. ambrosioides), and Group CO (Control-Blood clot). In each animal, bone defects measuring 2 mm in diameter were performed in both tibias for placement of the substances. After 7, 15, and 30 days, the animals were sedated and sacrificed using the cervical dislocation technique and the tissues were analyzed under optical microscope relative to the following events: inflammatory infiltrate, necrosis, osteoclasts, osteoblasts, fibroblasts, periosteal, and endosteal bone formation. The data were evaluated to verify distribution using the Kolmogorov-Smirnov test, and variance, using the Levene test; as distribution was not normal, data were subjected to the Kruskal-Wallis and Dunn nonparametric tests (p < .05). A significant inflammatory infiltrate was observed in Group CA5 (p = .008) in the time interval of 7 days, and in Group C at 15 (p = .009) and 30 (p = .017) days. Osteoblastic activity was more significant in Group CA20 (p = .027) compared with CA5 in the time interval of 7 days. Group CA20 demonstrated a significantly higher endosteal and periosteal bone formation value in the time interval of 7 (p = .013), 15 (p = .004), and 30 days (p = .008) compared with the other groups. The null hypothesis was refuted, bone regeneration was faster in spheres with an association of chitosan and 20% extract, and complete bone repair occurred clinically at 15 days and histologically at 30 days. The spheres proved to be a promising method for the biostimulation of alveolar bone repair and bone fractures.

Optimization of Epoxy Resin: An Investigation of Eggshell as a Synergic Filler.

Epoxy resin based on bisphenol A diglycidyl ether/anhydride methyl tetrahydrophthalic/2,4,6-tris(dimethylaminomethyl)phenol (DGEBA/MTHPA/DEH 35) was produced by magnetic stirring; chicken eggshell (ES) was added as cure improver. Thermal stability, cure parameters, mechanical properties, and fracture surface were investigated by thermogravimetry (TGA), differential scanning calorimetry (DSC), tensile experiments, and scanning electron microscopy (SEM). In general, the addition of ES slightly decreased the thermal stability, being T0.05 5% lower than that of the reference sample. The cure rate increased with the heating rates, while best results were obtained upon addition of neat membrane (M) from ES. Surprisingly, the mechanical properties were significantly improved with ES as well as with M, being the Young's modulus 18% higher, the tensile strength 50% higher, and the deformation 35% higher than those of epoxy resin. SEM images showed that the synthetic compounds presented a smooth fracture surface, while the compounds with ES and M had a rougher surface with multiplane fractures, suggesting a fracture with higher energy absorption. In conclusion, epoxy/ES composites with better performance were produced, and effective tools are provided to control and attain in the future even better properties with ecological features.

Physicomechanical and thermal analysis of bulk-fill and conventional composites.

The aim of this study was to evaluate the degree of conversion (DC) and the thermal stability of bulk-fill and conventional composite resins. Eleven composite resin samples were prepared to evaluate the DC, Vickers microhardness (VMH), mass and residue/particle loss, glass transition temperature (Tg), enthalpy, and linear coefficient of thermal expansion (CTE) using infrared spectroscopy (FTIR), microdurometer analyses, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dilatometry (DIL). The data were subjected to statistical analysis, with a significance level of 95%. DC and VMH were not influenced by the polymerized side of the sample, and statistical differences were recorded only among the materials. Decomposition temperature, melting, and mass and residue loss were dependent on the material and on the evaluation condition (polymerized and non-polymerized). Tg values were similar between the composites, without statistically significant difference, and CTE ranged from 10.5 to 37.1 (10-6/°C), with no statistical difference between the materials. There was a moderate negative correlation between CTE and the % of load particles, by weight. Most resins had a DC above that which is reported in the literature. TGA, Tg, and CTE analyses showed the thermal behavior of the evaluated composites, providing data for future research, assisting with the choice of material for direct or semidirect restorations, and helping choose the appropriate temperature for increasing the DC of such materials.

Role of Surfactants in the Properties of Poly(Ethylene Terephthalate)/Purified Clay Nanocomposites.

Purified clay was modified with different amounts of alkyl ammonium and phosphonium salts and used as filler in the preparation of PET nanocomposites via melt intercalation. The effect of this type of filler on morphology and thermal and mechanical properties of PET nanocomposites was investigated by X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analyses (TG), tensile properties, and transmission electron microscopy (TEM). The results showed that the mixture of alkyl ammonium and phosphonium salts favored the production of PET nanocomposites with intercalated and partially exfoliated morphologies with slight improvement in thermal stability. In addition, the incorporation of these organoclays tended to inhibit PET crystallization behavior, which is profitable in the production of transparent bottles.

Physicomechanical characterization and biological evaluation of bulk-fill composite resin.

The aim of this study was to evaluate the cytotoxic effect, degree of conversion (% DC), Vickers hardness (VH), and surface morphology of composite resins. Eleven resins, nine bulk-fill resins, and two conventional resins were evaluated. Each material was sampled to evaluate DC (using FTIR), VH, cytotoxicity (using MTT and Neutral Red - NR test), surface morphology (using SEM and AFM), and organic filler (using EDS). All statistical tests were performed with SPSS and the level of significance was set at 0.05. MTT revealed that the materials presented low or no cytotoxic potential in relation to the control. Opus was the resin with the lowest cell viability at a 1:2 concentration at 72 h (32%) and at 7 days (43%), but that significantly increased when the NR test was applied at a 1:2 concentration after 7 days. Thickness and surface subjected to polymerization had no influence on DC, and differences were observed only between the materials. In the microhardness test, statistical differences were observed between the evaluated thicknesses. The bulk-fill resins analyzed in this study exhibited low and/or no cytotoxicity to L929 cells, except for Opus, which showed moderate cytotoxicity according to the MTT assay. When the NR test was used, results were not satisfactory for all composites, indicating the need for different methodologies to evaluate the properties of these materials. The assessed resins demonstrated acceptable physicomechanical properties.

Physicomechanical and thermal analysis of bulk-fill and conventional composites

Abstract The aim of this study was to evaluate the degree of conversion (DC) and the thermal stability of bulk-fill and conventional composite resins. Eleven composite resin samples were prepared to evaluate the DC, Vickers microhardness (VMH), mass and residue/particle loss, glass transition temperature (Tg), enthalpy, and linear coefficient of thermal expansion (CTE) using infrared spectroscopy (FTIR), microdurometer analyses, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dilatometry (DIL). The data were subjected to statistical analysis, with a significance level of 95%. DC and VMH were not influenced by the polymerized side of the sample, and statistical differences were recorded only among the materials. Decomposition temperature, melting, and mass and residue loss were dependent on the material and on the evaluation condition (polymerized and non-polymerized). Tg values were similar between the composites, without statistically significant difference, and CTE ranged from 10.5 to 37.1 (10-6/°C), with no statistical difference between the materials. There was a moderate negative correlation between CTE and the % of load particles, by weight. Most resins had a DC above that which is reported in the literature. TGA, Tg, and CTE analyses showed the thermal behavior of the evaluated composites, providing data for future research, assisting with the choice of material for direct or semidirect restorations, and helping choose the appropriate temperature for increasing the DC of such materials.