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Scaffolds are devices with interconnected pores that favor cell interaction and proliferation. They play a significant role in tissue engineering, as they mimic the conditions of tissue production in vivo. The aim of this study was to synthesize scaffolds of chitosan, collagen, and Jatropha mollissima by lyophilization and characterize their chemical/biodegradability and morphological properties. For that, techniques of optical microscopy, infrared spectrometry, biodegradation test, and degree of swelling were performed. A 2% (m/v) chitosan/collagen (1:9) in lactic acid solution was produced. Then, Jatropha mollissima crude extract was added to this solution in different proportions of mass (5, 10, and 15%). Optical microscope images indicated the three-dimensional network formation with interconnected pores and predominantly lamellar shape. Through infrared spectrometry, characteristic bands indicated a physical mixture. Also, the swelling degree of all samples was proportional to the amount of Jatropha mollissima extract with the highest percentage of 1852%. Biodegradation test also revealed a proportional ratio between the amount of sap used and the degraded percentage with the lowest value of around 35% in 28 days. In conclusion, it can be inferred that the scaffolds produced show potential to be used in tissue engineering as dressings.

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.

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.

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.

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.

Abstract Poly(ether ether ketone) (PEEK) has excellent properties, such as high biocompatibility and an elastic modulus similar to bone, which makes it a suitable biomaterial. When modified with sulfuric acid (H2SO4) and hydroxyapatite (HA), its workability and bioactivity is enhanced, and this makes it of great importance in medicine. This study investigates a better combination of process parameters to manufacture sulfonated PEEK/HA (SPEEK/HA) membranes for biomaterials. Chemical, thermal, and biological analyses were carried out on all samples. The sulfonated structure was observed to enhance wettability, adhesion, and cell viability. Furthermore, an increase in the degree of sulfonation facilitated their workability as required for biomaterials; making them suitable for osseointegration. Besides, the SPEEK/HA membranes presented cell adhesion, confirming the viability to use as biomaterial. This study presents a cheap alternative method to easily process biomaterials of improved workability.

Carbonated hydroxyapatite (CHAp) and β-tricalcium phosphate (β-TCP) have been employed for decades as constituents of scaffolds for bone regeneration because they chemically resemble bone mineral. In this study, the feasibility to manufacture CHAp/β-TCP scaffolds by pseudomorphic transformation of casted blocks of gypsum was investigated. The transformation was carried out by immersing the precursor gypsum block in 1 M (NH4)2HPO4/1.33 M NH4OH solution with liquid/solid ratio of 10 mL/g and autoclaving at 120 °C and 203 kPa (2 atm) for 3 h at least. Neither shape nor dimensions significantly changed during transformation. The composition of scaffolds treated for 3 h was 70 wt.% CHAp and 30 wt.% β-TCP, and their compressive and diametral compressive strengths were 6.5 ± 0.7 and 5.3 ± 0.7 MPa, respectively. By increasing the time of treatment to 6 h, the composition of the scaffold enriched in β-TCP (60 wt.% CHAp and 40 wt.% β-TCP) but its compressive and diametral compressive strengths were not significantly affected (6.7 ± 0.9 and 5.4 ± 0.6 MPa, respectively). On the basis of the results obtained, it was concluded that this route is a good approach to the manufacturing of biphasic (CHAp/β-TCP) scaffolds from previously shaped pieces of gypsum.

Nanoparticles of zinc oxide (ZnO) were added to poly( ε -caprolactone) (PCL), and PCL/ZnO casting films were produced, afterwards films were characterized using Fourier Transform Infrared Spectroscopy (FTIR), x-ray Diffraction (XRD), Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM). Additionally, antimicrobial and cytotoxic parameters were determined using microbial adhesion testing according to JIS Z 2801: 2000 (E) and agar diffusion method according to ISO 10993-5 2009 , respectively. From collected data, the chemical identity of individual components was kept and the surface control could be achieved changing the composition. According to FTIR spectra and using the Lambert-Beer law higher interaction ratios were met for higher ZnO content which is linked to antimicrobial action. As revealed by AFM analysis, at 5% of ZnO, nanoparticles were well dispersed in PCL matrix with uniform surface film. Analyses from antibacterial activity and cytotoxicity suggested pathogenic Staphylococcus aureus growth was hindered in ZnO films; specifically for PCL/ZnO 5% optimal antibacterial activity and toxicity absent were reached. Summing up, PCL/ZnO5% nanocomposites films offer great potential for commercial applications as active food packaging.

Abstract 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.

The aim of this work was to perform an analysis of the influence of Sodium Fluoride (NaF) on chitosan particles size and morphology produced via ionotropic gelation with higher rotational stirring speed. Samples were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Dynamic Light Scattering (DLS), Zeta Potential (ζ), Scanning Electron Microscopy and Energy Dispersive Spectroscopy (SEM/EDS). Chitosan/TPP particles diameter obtained was in the order of 3.8 µm. When NaF was added in different concentration (0.05%, 0.2% and 2%), the particle size diameter values, Zeta Potential and Poly Dispersive Index measures consequently decreased. Even so, no further modification in morphology was found. An exception was made for the samples with higher NaF concentration. After 21 days, occurred an increase in the particle size diameter. In the future, the proposed methodology could provide a dentistry application, especially on delivering particles of NaF.

Several studies have established an association between diabetes and alterations in bone metabolism; however, the underlying mechanism is not well established. Although zinc is recognized as a potential preventive agent against diabetes-induced bone loss, there is no evidence demonstrating its effect in chronic diabetic conditions. This study evaluated the effects of zinc supplementation in a chronic (90 days) type 1 diabetes-induced bone-loss model. Male Wistar rats were distributed in three groups: control, type 1 diabetes mellitus (T1DM), and T1DM plus zinc supplementation (T1DMS). Serum biochemical analysis; tibia histomorphometric, biomechanical, and collagen-content analyses; and femur mRNA expression were evaluated. Relative to T1DM, the zinc-supplemented group showed increased histomorphometric parameters such as TbWi and BAr and decreased TbSp, increased biomechanical parameters (maximum load, stiffness, ultimate strain, and Young's modulus), and increased type I collagen content. Interestingly, similar values for these parameters were observed between the T1DMS and control groups. These results demonstrate the protective effect of zinc on the maintenance of bone strength and flexibility. In addition, downregulation of OPG, COL1A, and MMP-9 genes was observed in T1DMS, and the anabolic effects of zinc were evidenced by increased OC expression and serum ALP activity, both related to osteoblastogenesis, demonstrating a positive effect on bone formation. In contrast, T1DM showed excessive bone loss, observed through reduced histomorphometric and biomechanical parameters, characterizing diabetes-associated bone loss. The bone loss was also observed through upregulation of OPG, COL1A, and MMP-9 genes. In conclusion, zinc showed a positive effect on the maintenance of bone architecture and biomechanical parameters. Indeed, OC upregulation and control of expression of OPG, COL1A, and MMP-9 mRNAs, even in chronic hyperglycemia, support an anabolic and protective effect of zinc under chronic diabetic conditions. Furthermore, these results indicate that zinc supplementation could act as a complementary therapy in chronic T1DM.

Abstract Background Evidence suggests that semi-facial respirators provide protection against contamination in high-risk environments, although the COVID-19 pandemic called for greater protection and viral inactivation capacity. Thus, the aim of this study was to investigate the efficacy of a novel semi-facial respirator containing chitosan nanoparticles, compared with a conventional N95 respirator on the incidence of laboratory-confirmed SARS-CoV-2 in healthcare professionals. The secondary outcomes were influenza infection, usability and comfort. Methods Randomized controlled trial within a large public hospital (reference for COVID-19 patients) carried out between March 2021 and June 2023. We included 230 healthcare professionals exposed to SARS-Cov-2 and influenza, working in emergency departments, hospital wards, and intensive care units. Participants were assessed at baseline, after 10 days, and 21 days of follow-up. Researchers, participants, and outcome assessors were blinded to the allocated groups. Outcomes were analyzed by bivariate and multivariate comparisons using logistic regression. Crude (cOR) and adjusted odds ratios (aOR) were estimated, followed by 95% confidence intervals (CIs 95%). We adopted intention-to-treat (ITT) and complete-case (CC) analyses. Results Baseline characteristics were considered homogeneous between groups, and usability and comfort were reported as excellent in both groups. Non-significant differences were found for all outcomes, both in the ITT and CC analyses. The incidence of COVID-19 and influenza were, respectively, cOR: 0.96 [CI95%: 0.21–4.42] and cOR: 1.25 [CI95%: 0.34–4.62]; and aOR: 1.08 [CI95%: 0.21–5.47] and aOR: 1.11 [CI95%: 0.17–7.01]. Conclusions We found that the incidence of SARS-Cov-2 and influenza infections were similar between the new respirator compared to the conventional respirator. Furthermore, we observed that usability and comfort were similar and considered excellent for both respirators. Trial registration Clinicaltrials.gov (NCT04490200, 29/07/2020).

The aim of this study was to develop a material capable of rapidly absorbing bodily fluids and forming a resilient, adhesive, viscoelastic hydrogel in situ to prevent post-surgical adhesions. This material was formulated using O-carboxymethyl chitosan (O-CMCS), oxidized hyaluronic acid (OHA), and a crosslinking pigment derived from genipin and glutamic acid (G/GluP). Both crosslinked (O-CMCS/OHA-G/GluP) and non-crosslinked hydrogels (O-CMCS/OHA) were evaluated using a HAAKE™ MARS™ rheometer for their potential as post-surgical barriers. A rheological analysis, including dynamic oscillatory measurements, revealed that the crosslinked hydrogels exhibited significantly higher elastic moduli (G′), indicating superior gel formation and mechanical stability compared to non-crosslinked hydrogels. The G/GluP crosslinker enhanced gel stability by increasing the separation between G′ and G″ and achieving a lower loss tangent (tan δ < 1.0), indicating robustness under dynamic physiological conditions. The rapid hydration and gelation properties of the hydrogels underscore their effectiveness as physical barriers. Furthermore, the O-CMCS/OHA-G/GluP hydrogel demonstrated rapid self-healing and efficient application via spraying or spreading, with tissue adherence and viscoelasticity to facilitate movement between tissues and organs, effectively preventing adhesions. Additionally, the hydrogel proved to be both cost effective and scalable, highlighting its potential for clinical applications aimed at preventing post-surgical adhesions.

Abstract 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.

Abstract With the rising in life expectancy and the consequent population aging, degenerative chronic diseases have been figured as the major cause of morbidity and mortality in the world. It is believed that the production of a polymeric matrix composed of chitosan and gelatin may be an alternative to obtain a carrier base of heparin, with the prospective objective of applying these materials as an alternative to the conventional therapeutic resources biomedical. Based on the results, it can be concluded that the interaction between chitosan, gelatin, and heparin demonstrating a satisfactory result by the methodologies that were applied, making the study hypothesis concrete., certifying the use of a methodology for including heparin in a biodegradable polymeric base. Thus, expanding the alternatives for possible alternatives to the conventional therapeutic resources of vascular diseases with the application of the developed 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.

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.

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.

O uso de pontas diamantadas de forma descartável tem sido incentivado, porém a re-esterilização é uma prática habitual nos consultórios odontológicos. O objetivo deste estudo piloto é verificar, por meio da microscopia eletrônica de varredura (MEV), as alterações nas características superficiais de pontas diamantadas devido ao método de esterilização através do uso da autoclave (calor úmido). Foram utilizadas 3 pontas diamantadas 1014 da marca MICRODONT®, às quais foram submetidas a diferentes procedimentos, sendo P1 (Ponta 1) não submetida a nenhum ciclo de esterilização, sendo, portanto, o controle; P2 (Ponta 2) submetida a esterilização através do calor úmido em autoclave por 5 vezes consecutivas e P3 (Ponta 3) submetida por 10 vezes consecutivas à esterilização em autoclave. Posteriormente as pontas diamantadas foram analisadas por microscopia eletrônica de varredura (MEV), utilizando-se aumentos de 150x, 330x e 500x. Observou-se que as pontas utilizadas nesta pesquisa, às quais foram submetidas à esterilização, sofreram desgaste por corrosão, sendo que a ponta submetida a 10 ciclos consecutivos de esterilização apresentou um maior desgaste. É possível concluir que a corrosão sofrida pelas pontas devido ao processo de esterilização em autoclave ocasiona a perda de grãos de diamante o que pode acarretar em queda no seu desempenho de corte, prejudicando sua eficiência.

Polyetheretherketone (PEEK) has been prominent in orthopedic implants; however, it is inert, preventing interaction between the implant and adjacent bone tissues. One way to overcome this characteristic is physical modification its on surface by particle leaching promoting greater osseointegration. The objective of this research was to develop and characterize the PEEK using a surface modification technique via particle leaching. For of the samples, a layer deposition of NaCl was used on PEEK. This was subjected to the pressure of 850 kg/cm2 by 390ºC for 20 minutes. After cooling, were subjected to leaching process particles. The results indicated a porous surface exhibiting uniform and homogeneous morphology with defined pores interconected, to in the range of 140-373 µm, with an average diameter of 273 µm. These evidenced the considerable NaCl removal after the leaching process, with cavities from ideal sizes which promotes adequate cellular accommodation and distinct roughness, giving an overall possibility of being able to obtain a material more able to receive the cells while also possibly presenting cell viability. Although the compressive strength presented low values, it can still be suitable for applications in areas with a reduced modulus of elasticity.

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.

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.

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.

The aim of this study was to develop an inexpensive apparatus for fabricating microspheres, based on chitosan, for 5-fluorouracil (5-FU) controlled release. Chitosan microspheres were prepared by precipitation method and the effects of manufacturing parameters (injection and airflow rates) on size distribution microspheres were analyzed by optical and scanning electron microscopy. The results show that the manufacturing parameters, injection and airflow rates, determine the microsphere size distribution. By modulating these parameters, it was possible to produce chitosan microspheres as small as 437 ± 44 μm and as large as 993 ± 18 μm. Chitosan microspheres loaded with 5-FU were also produced using the experimental equipment. The obtained microspheres presented 5-FU controlled release, indicating that the microspheres can be used orally, since they are capable of crossing the stomach barrier and of continuing with the process of 5-FU release.

Film-forming emulsions and films, prepared by incorporating different concentrations of clove essential oil (CEO) and melaleuca essential oil (MEO) into chitosan (CS) were obtained and their properties were evaluated. Film-forming emulsions were characterized in terms of qualitative assessment, hydrogen potential and in vitro antibacterial activity, that was carried by the agar diffusion method, and the growth inhibition effects were tested on the Gram-positive microorganism of Staphylococcus aureus, Gram-negative microorganisms of Escherichia coli, and against isolated fungi such as Candida albicans. In order to study the impact of the incorporation of CEO and MEO into the CS matrix, the appearance and thickness of the films were evaluated. Furthermore, Fourier transform infrared spectroscopy (FTIR), contact angle measurements, a swelling test, scanning electron microscopy and a tensile test were carried out. Results showed that the film-forming emulsions had translucent aspect with cloudy milky appearance and showed antimicrobial properties. The CEO had the highest inhibition against the three strains studied. As regards the films’ properties, the coloration of the films was affected by the type and concentration of bioactive used. The chitosan/CEO films showed an intense yellowish coloration while the chitosan/MEO films presented a slightly yellowish coloration, but in general, all chitosan/EOs films presented good transparency in visible light besides flexibility, mechanical resistance when touched, smaller thicknesses than the dermis and higher wettability than chitosan films, in both distilled water and phosphate-buffered saline (PBS). The interactions between the chitosan and EOs were confirmed by. The chitosan/EOs films presented morphologies with rough appearance and with EOs droplets in varying shapes and sizes, well distributed along the surface of the films, and the tensile properties were compatible to be applied as wound dressings. These results revealed that the CEO and MEO have a good potential to be incorporated into chitosan to make films for wound-healing applications.

The aim of this study was to prepare chitosan (CS) filaments incorporated with N-acetyl-D-Glucosamine (GlcNAc), using the wet spinning method, in order to combine the GlcNAc pharmacological properties with the CS biological properties for use as absorbable suture materials. The filaments were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), uniaxial tensile testing, in vitro biodegradation, and through in vitro drug release and cytotoxicity studies. It was observed that the addition of GlcNAc did not alter the morphology of the filaments. The CS and CS/GlcNAc filaments presented diameters 145 µm and 148 µm, respectively, and the surfaces were homogeneous. Although the mechanical resistance of the chitosan filaments decreased with the incorporation of the GlcNAc drug, this property was greater than the mean values indicated in the U.S. Pharmacopeia (1.7 N) for suture number 6-0 (filament diameter of 100−149 μm). The biodegradation of the CS filaments was accelerated by the addition of GlcNAc. After 35 days, the CS/GlcNAc filaments degradability was at its total, and for the CS filaments it was acquired in 49 days. The in vitro kinetic of the release process was of the zero-order and Hopfenberg models, controlled by both diffusion and erosion process. The in vitro cytotoxicity data of the CS and CS/GlcNAc filaments toward L929 cells showed that these filaments are nontoxic to these cells. Thus, the GlcNAc-loaded CS filaments might be promising as absorbable suture materials. In addition, this medical device may be able to enhance healing processes, relieve pain, and minimize infection at the surgery site due the prolonged release of GlcNAc.

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.

This work aimed to prepare chitosan/clay microspheres, by the precipitation method, for use in drug carrier systems. The influence of the process parameters, particularly two airflows of the drag system (2.5 and 10 L·min−1) on the microspheres physical dimensions and properties, such as microstructure, degree of swelling and porosity were evaluated. The samples were characterized by optical microscopy (OM), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Water absorption and porosity tests were also performed. The results showed that the process parameters affected the size of the microspheres. The diameter, volume and surface area of the chitosan/clay microspheres decreased when they were prepared with the higher airflow of the drag system. The microspheres presented a porous microstructure, being the pore size, percentage of porosity and degree of swelling affected not only by the process parameters but also by the type of clay. Hybrids (chitosan/clay) with intercalated morphology were obtained and the hybrid prepared with montmorillonite clay at higher airflows of the drag system presented the greatest interlayer spacing and a more disordered morphology. Thus, it is certain that the chitosan/clay nanocomposite microspheres prepared with montmorillonite (CL clay) at higher airflows of the drag system can have good drug-controlled release properties.

O objetivo do presente trabalho foi avaliar o processo de regeneração óssea em coelhos através da utilização da hidroxiapatita e da quitosana isoladas e associadas à medula óssea. Foram utilizados 20 coelhos adultos, de ambos os sexos, da raça Nova Zelândia e pesando em média 3,0±0,4kg. Os animais foram divididos ao acaso de acordo com dois momentos experimentais, sendo que 10 animais foram submetidos à eutanásia 30 dias após a cirurgia, e 10, 60 dias após a cirurgia. Foram utilizados quatro implantes que constituíram os grupos. Os materiais foram introduzidos em defeitos criados cirurgicamente na metáfise proximal (MP) e distal (MD) de cada fêmur, de modo que a quitosana foi introduzida na MP e a hidroxiapatita na MD do membro esquerdo e, no membro direito, além dos implantes, foi adicionada medula óssea. Na avaliação histológica descritiva comparativa, constatou-se que os grupos QUI e QUIMO, em ambos os momentos estudados, estimularam reações mais acentuadas e aceleraram o reparo ósseo. Na análise morfométrica, os grupos QUI e QUIMO diferiram estatisticamente dos outros grupos, tendo sido observada maior formação óssea (P

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.

The crystallization of hydroxyapatite (HA) in aqueous solution can be described by the mechanism ACP -> OCP -> HA. In this work, it was studied the influence of K+, Mg2+, SO4(2-) and CO3(2-) ions in the formation of ACP and in its conversion to OCP, using biomimetic coatings on metallic substrates of commercially pure titanium (Ti c.p.). The results showed that Mg2+ and CO3(2-) ions favored both the formation of ACP and its conversion to OCP. Differently, K+ and SO4(2-) ions did not influence the formation of ACP and, consequently, interfered in the conversion to OCP.

Commercial purity titanium (cp-Ti), and some of its alloys are important materials in the medical field because of their excellent biocompatibility and mechanical properties. Recently a simple chemical method to induce bioactivity in these inert metallic materials was reported. In this work, the biomimetic chemical process has been used to modify the surface of cp-Ti with the formation of a deposit layer of apatite (a calcium phosphate compound). The main purpose was to study the influence of heat treatment on changes in crystallinity in the deposited phases. X-ray diffraction analysis and scanning electron microscopy showed that the apatite coatings heat treated between 400 and 600 °C were less crystalline, similar to biological apatites. Upon heat treatment at temperatures above 700 °C, the apatite coatings appeared more crystalline, and were a mixture of hydroxyapatite, octacalcium phosphate and magnesium phosphate.

The main source of commercial chitosan is the extensive deacetylation of its parent polymer chitin. It is present in green algae, the cell walls or fungi and in the exoskeleton of crustaceans. A novel procedure for preparing chitosan from shrimp shells was developed. The procedure involves two 10-minutes bleaching steps with ethanol after the usual demineralization and deproteinization processes. Before deacetylation, chitin was immersed in 12.5 M NaOH, cooled down and kept frozen for 24 h. The obtained chitosan was characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV, X-ray diffraction (XRD) and viscosimetry. Samples of white chitosan with acetylation degrees below 9 % were obtained, as determined by FTIR and UV-first derivative spectroscopy. The change in the morphology of samples was followed by SEM. The ash content of chitosan samples were all below 0.063 % . Chitosan was soluble in 1 % acetic acid with insoluble contents of 0.62 % or less. XRD patterns exhibited the characteristic peaks of chitosan centered at 10 and 20 degrees in 2 θ . The molecular weight of chitosan was between 2.3 and 2.8 × 10 5 g/mol. It is concluded that the procedure developed in the present work allowed obtaining chitosans with physical and chemical properties suitable for pharmaceutical applications.

O objetivo deste estudo foi avaliar os fosfatos de cálcio, pirofosfato de cálcio (CPP) com tratamento térmico a 700 e 900°C, fosfato tricálcio associado à hidroxiapatita (TCP/HA) e hidroxiapatita (HA) como substitutos ósseos. Foram utilizados 20 coelhos (Oryctolagus cuniculus), de ambos os sexos, da raça Nova Zelândia, pesando em média 2,5±0,41kg. Os animais foram distribuídos, ao acaso, em dois grupos de 10 animais de acordo com o período em que foram eutanasiados (30 ou 60 dias). Os implantes foram introduzidos na metáfise proximal e distal de cada fêmur, de modo que os CPP 700 e 900 foram introduzidos no membro esquerdo, enquanto o TCP/HA e HA no membro direito. Foram realizadas avaliações clínico-cirúrgicas e radiográficas imediatamente após a cirurgia e aos 30 e 60 dias do pós-operatório. Os animais apresentaram evolução clínica normal. Na avaliação radiográfica observou-se diferença estatística entre os grupos com maior grau de radiopacidade nos animais do grupo 60 dias que utilizaram os implantes TCP/HA e HA. Na avaliação histológica, por meio de microscopia de luz e análise morfométrica, os materiais TCP/HA e HA proporcionaram maior neoformação óssea ao redor dos implantes do que com os CPP700 e CPP900 aos 30 e 60 dias de avaliação.