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Corrosion performance of polypyrrole-bilayer coating on carbon steel
(Springer Nature) Cho, Liu Yao; Guiotti, Luciano Grande; Liu, Andrea Santos
Polypyrrole doped with phosphoric acid was electrochemically synthesized on carbon steel from acetonitrile medium, and then a coating of polypyrrole doped with a long carbon chain acid, dodecylbenzenesulfonic acid or lauric acid, was electrodeposited to form a bilayer. The more protective performance of the bilayers in relation to monolayers was explained in terms of adherence and low porous, as confirmed by scanning electron microscopy. The corrosion perfor- mance was also confirmed by electrochemical measurements of open-circuit potential, potentiodynamic polarization curves and electrochemical impedance spectroscopy in chloride solution. The polarization experiments indicated that the corrosion potential values for polypyrrole-bilayer-coated steel were shifted to the positive direction in relation to uncoated carbon steel, indicating anodic protection. Tafel plots also indicated that the anodic current densities were smaller for steel coated by polypyrrole-bilayer. In addition, the electrochemical impedance data showed that the charge transfer resistance values are associated with the resistance to electron exchange between the metal and the coating, and depend on the type of long carbon chain dopant used in the outer-layer. Thus, the suggested mechanism to explain the protection of carbon steel surfaces against corrosion was associated to the passivation and barrier effect of the polypyrrole-bilayer.
Scratch and wear behaviour of Co-Cr-Mo alloy in ringer’s lactate solution
(MDPI) Silva, Raimundo; Santos, Marcos Dantas dos; Madureira, Rui; Soares, Rui; Neto, Rui; Vieira, Angela Aparecida; Gonçalves, Polyana Alves Radi; Leite, Priscila Maria Sarmeiro M.; Vieira, Lúcia; Viana, Filomena
Cobalt–chromium–molybdenum (Co-Cr-Mo) alloy is a material recommended for biomedical implants; however, to be suitable for this application, it should have good tribological properties, which are related to grain size. This paper investigates the tribological behaviour of a Co-Cr-Mo alloy produced using investment casting, together with electromagnetic stirring, to reduce its grain size. The samples were subjected to wear and scratch tests in simulated body fluid (Ringer’s lactate solution). Since a reduction in grain size can influence the behaviour of the material, in terms of resistance and tribological response, four samples with different grain sizes were produced for use in our investigation of the behaviour of the alloy, in which we considered the friction coefficient, wear, and scratch resistance. The experiments were performed using a tribometer, with mean values for the friction coefficient, normal load, and tangential force acquired and recorded by the software. Spheres of Ti-6Al-4V and 316L steel were used as counterface materials. In addition, to elucidate the influence of grain size on the mechanical properties of the alloy, observations were conducted via scanning electron microscopy (SEM) with electron backscatter diffraction (EBSD). The results showed changes in the structure, with a reduction in grain size from 5.51 to 0.79 mm. Using both spheres, the best results for the friction coefficient and wear volume corresponded to the sample with the smallest grain size of 0.79 mm. The friction coefficients obtained were 0.37 and 0.45, using the Ti-6Al-4V and 316L spheres, respectively. These results confirm that the best surface finish for Co-Cr-Mo alloy used as a biomedical implant is one with a smaller grain size, since this results in a lower friction coefficient and low wear.
Molhabilidade de não tecido eletrofiado contendo nanopartículas de prata para uso em filtro
(Faculdade Senai Roberto Mange) Shimada, Yoshio Manoel Nunes; Silva, Daniele Cristina; Bustamante, Gabriel Costa; Vieira, Angela Aparecida; Gonçalves, Erika Peterson; Vieira, Lucia
Sabe-se que hospitais podem ser ambientes endêmicos onde a coinfecção por vírus e bactérias pode ocorrer. O uso de novos materiais e métodos de processamento para fabricar filtros ou máscaras ocorrem devido à sua ampla aplicação. Para este estudo, um sistema de eletrofiação foi usado para fabricar não tecidos baseados em fibras de poliacrilonitrila (PAN), com e sem a adição de nanopartículas de prata (Ag). Após a produção, as amostras receberam um tratamento térmico em atmosfera de nitrogênio, a fim de reduzir o efeito eletrostático. Os materiais foram avaliados em termos de molhabilidade pela medição de ângulo de contato. Para a análise da morfologia das fibras, foram usadas microscopia eletrônica de varredura e transmissão. Os testes de molhabilidade mostraram que o PAN+Ag possuí características hidrofóbicas, de acordo com as recomendações para filtros de proteção pessoal sendo capaz de reter gotículas e aerossóis.
Crystalline structure, morphology, and adherence of thick TiO2 films grown on 304 and 316L stainless steels by atomic layer deposition
(MDPI) Marques, Vagner Eduardo Caetano; Manfroi, Lucas Augusto; Vieira, Angela Aparecida; Pereira, André Luis de Jesús; Marques, Francisco das Chagas; Vieira, Lúcia
Titanium dioxide (TiO2) thin films are widely used in transparent optoelectronic devices due to their excellent properties, as well as in photocatalysis, cosmetics, and many other biomedical applications. In this work, TiO2 thin films were deposited onto AISI 304 and AISI 316L stainless steel substrates by atomic layer deposition, followed by comparative evaluation of the mixture of anatase and rutile phase by X-ray diffraction, Raman maps, morphology by SEM-FEG-AFM, and adhesion of the films on the two substrates, aiming to evaluate the scratch resistance. Raman spectroscopy mapping and X-ray diffraction with Rietveld refinement showed that the films were composed of anatase and rutile phases, in different percentages. Scratch testing using a diamond tip on the TiO2 film was employed to evaluate the film adherence and to determine the friction coefficient, with the results showing satisfactory adherence of the films on both substrates.
Biocomposite macrospheres based on strontium-bioactive glass for application as bone fillers
(American Chemical Society) Oliveira, Ivone Regina de; Gonçalves, Isabela dos Santos; Santos, Kennedy Wallace dos; Lança, Maria Carmo; Vieira, Tânia; Silva, Jorge Carvalho; Cengiz, Ibrahim Fatih; Reis, Rui Luís; Oliveira, Joaquim Miguel; Borges, João Paulo Miranda Ribeiro
Traditional bioactive glass powders are typically composed of irregular particles that can be packed into dense configurations presenting low interconnectivity, which can limit bone ingrowth. The use of novel biocomposite sphere formulations comprising bioactive factors as bone fillers are most advantageous, as it simultaneously allows for packing the particles in a 3-dimensional manner to achieve an adequate interconnected porosity, enhanced biological performance, and ultimately a superior new bone formation. In this work, we develop and characterize novel biocomposite macrospheres of Sr-bioactive glass using sodium alginate, polylactic acid (PLA), and chitosan (CH) as encapsulating materials for finding applications as bone fillers. The biocomposite macrospheres that were obtained using PLA have a larger size distribution and higher porosity and an interconnectivity of 99.7%. Loose apatite particles were observed on the surface of macrospheres prepared with alginate and CH by means of soaking into a simulated body fluid (SBF) for 7 days. A dense apatite layer was formed on the biocomposite macrospheres’ surface produced with PLA, which served to protect PLA from degradation. In vitro investigations demonstrated that biocomposite macrospheres had minimal cytotoxic effects on a human osteosarcoma cell line (SaOS-2 cells). However, the accelerated degradation of PLA due to the degradation of bioactive glass may account for the observed decrease in SaOS-2 cells viability. Among the biocomposite macrospheres, those composed of PLA exhibited the most promising characteristics for their potential use as fillers in bone tissue repair applications.
Zinc pthalocyanine loaded poly (lactic acid) nanoparticles by double emulsion methodology for photodynamic therapy against 9 L/LacZ gliosarcoma cells
(Taylor & Francis Group) Oliveira Junior, Benedito Marcio de; Teodoro, Jéssica Beatriz Miranda; Ambrósio, Jéssica Aparecida Ribeiro; Gonçalves, Érika Peterson; Beltrame Junior, Milton; Marcolino, Luciana Maria Cortez; Pinto, Juliana Guerra; Ferreira-Strixino, Juliana; Simioni, Andreza Ribeiro
Development delivery systems, such as nanoparticles, represent a growing area in biomedical research. Nanoparticles (NP) were prepared using a double-emulsion method to load zinc(II) phthalocyanine (ZnPc). NP were obtained using poly (lactic acid) (PLA). ZnPc is a second generation of photosensitizer used in photodynamic therapy (PDT). ZnPc loaded PLA nanoparticles (NPLAZnPc) were prepared by double-emulsion method, characterized and available in cellular culture. The mean nanoparticle size presented particle size was 384.7 ± 84.2 nm with polydispersity index (PDI) of 0.150 ± 0.015, and the encapsulation efficiency was of 83%. The nanoparticle formulations presented negative zeta potential values (27.5 ± 1.0 mV), explaining their colloidal stability. ZnPc loaded nanoparticles maintain its photophysical behavior after encapsulation. Photosensitizer release from nanoparticles was sustained over 168 h with a biphasic ZnPc release profile. An in vitro phototoxic effect in range of 80% was observed in 9 L/ LacZ gliosarcoma cells at laser light doses (10 J cm2) with 3.0 mg mL1 of NPLA-ZnPc. All the physical–chemical, photophysical and photobiological measurements performed allow us to conclude that ZnPc loaded PLGA nanoparticles is a promising drug deliverysystem for PDT.
Synthesis and characterization of photosensitive gelatin-based hydrogels for photodynamic therapy in HeLa-CCL2 cell line
(Elsevier) Ambrósio, Jéssica Aparecida Ribeiro; Pinto, Bruna Cristina dos Santos; Marmo, Vitor Luca Moura; Santos, Kennedy Wallace dos; Beltrame Junior, Milton; Pinto, Juliana Guerra; Ferreira-Strixino, Juliana; Raniero, Leandro José; Simioni, Andreza Ribeiro
Background: Hydrogel systems are increasingly gaining visibility involving biomedicine, tissue engineering, environmental treatments, and drug delivery systems. These systems have a three-dimensional network composition and high-water absorption capacity, are biocompatible, allowing them to become an option as photosensitizer carriers (PS) for applications in Photodynamic Therapy (PDT) protocols. Methods: A nanohydrogel system (NAHI), encapsulated with chloroaluminium phthalocyanine (ClAlPc) was synthesized for drug delivery.. NAHI was synthesized using gelatin as based polymer by the chemical cross-linking technique. The drug was encapsulated by immersing the hydrogel in a 1.0 mg.mL􀀀 1 ClAlPc solution. The external morphology of NAHI was examined by scanning electron microscopy (SEM). The degree of swelling of the synthesized system was evaluated to determine the water absorption potential. The produced nanohydrogel system was characterized by photochemical, photophysical and photobiologial studies. Results: The images from the SEM analysis showed the presence of three-dimensional networks in the formulation. The swelling test demonstrated that the nanohydrogel freeze-drying process increases its water holding capacity. All spectroscopic results showed excellent photophysical parameters of the drug studied when served in the NAHI system. The incorporation efficiency was 70%. The results of trypan blue exclusion test have shown significant reduction (p < 0.05) in the cell viability for all groups treated with PDT, in all concentrations tested. In HeLa cells, PDT mediated by 0,5 mg.mL􀀀 1 ClAlPc encapsulated in NAHI showed a decrease in survival close to 95%. In the internalization cell study was possible to observe the internalization of phthalocyanine after one hour of incubation, at 37 ◦C, with the the accumulation of PS in the cytoplasm and inside the nucleus at both concentrations tested. Conclusions: Given the peculiar performance of the selected system, the resulting nanohydrogel is a versatile platform and display potential applications as controlled delivery systems of photosensitizer for photodynamic therapy application.
Synthesis, characterization, and evaluation of chloroaluminium phthalocyanine incorporated in poly(ε-caprolactone) nanoparticles for photodynamic therapy
(Elsevier) Pinto, Bruna Cristina dos Santos; Ambrósio, Jéssica Aparecida Ribeiro; Marmo, Vitor Luca Moura; Pinto, Juliana Guerra; Raniero, Leandro José; Ferreira-Strixino, Juliana; Simioni, Andreza Ribeiro; Beltrame Junior, Milton
Background: The use of nanotechnology has been widely used in biomedical science, including orthopedic implants, tissue engineering, cancer therapy and drug elution from nanoparticle systems, such as poly-caprolactone (PCL) nanoparticles, which stand out mainly for their biocompatibility, being considered as effective carriers for photosensitizing drugs (PS) in photodynamic therapy (PDT) protocols. Methods: This manuscript describes the synthesis and characterization of PCL nanoparticles for controlled release of the drug chloro-aluminum phthalocyanine (ClAlPc) as a photosensitizer for application in PDT. The PCL-ClAlPc nanoparticles were developed by the nanoprecipitation process. The structure and morphology of the nanoparticles were studied with scanning electron microscopy (SEM) and with Fourier transform infrared (FTIR). The size of nanomaterials was studied using the Dynamic Light Scattering (DLS) method. Photophysical and photochemical characterizations were performed. Subsequently, photobiological studies were also used to characterize the system. Results: The nanoparticles had an average diameter of 384.7 ± 138.6 nm and a polydispersity index of 0.153. SEM analysis revealed that the system formed a spherical shape typical of these delivery systems. Charging efficiency was 82.1% ± 1.2%. The phthalocyanine-loaded PCL nanoparticles maintained their photophysical behavior after encapsulation. Cell viability was determined after the dark toxicity test, and it was possible to observe that there was no evidence of toxicity in the dark, for all concentrations tested. The assay also revealed that adenocarcinoma cells treated with free ClAlPc and in the nanoformulation showed 100% cell death when subjected to PDT protocols. The intracellular location of the photosensitizer indicated a high potential for accumulation in the cytoplasm and nucleus. Conclusions: From the photophysical, photochemical and photobiological analyzes obtained, it was possible to observe that the development of PCL nanoparticles encapsulated with ClAlPc, by the nanoprecipitation method was adequate and that the in vivo release study is efficient to reduce the release rate and attenuate the burst of PS loaded on PCL nanoparticles. The results reinforce that the use of this system as drug delivery systems is useful in PDT protocols.
Zinc phthalocyanine tetrasulfonate-loaded polyelectrolytic PLGA nanoparticles for photodynamic therapy applications
(Elsevier) Toledo, Maria Cristina Modesto Clementino de; Abreu, Alexandro da Silva; Carvalho, Janicy Arantes; Ambrósio, Jéssica Aparecida Ribeiro; Godoy, Daniele da Silva; Pinto, Bruna Cristina dos Santos; Beltrame Junior, Milton; Simioni, Andreza Ribeiro
Background: Photodynamic Therapy (PDT) is a modality for the treatment of neoplastic tissues, which is based on the administration of a phototherapeutic agent and light irradiation at an appropriate wavelength, aiming to locate and destroy the target cell with the formation of reactive oxygen species. Nanoencapsulation technology presents itself as a tool for incorporation of bioactive substances aiming to improve their solubility in physiological environment, obtain a longer circulation time in the organism, administration of lower dosages and the minimization of side effects. The present work aimed at the development of poly (lactic acid-glycolic acid) (PLGA) nanoparticles coated with polyelectrolyte film layers for encapsulating zinc phthalocyanine tetrasulfonated (ZnPcSO4) as a bioactive substance model. Methods: PLGA nanoparticles were produced by the double emulsion/solvent evaporation technique and polyelectrolytic coating was performed using polyalkylamine hydrochloride (PAH) as a weak polycation and poly (4- styrene sulfonate) (PSS) as a strong polyanion by layer-by-layer self-assembly technique (known as layer-by-layer-LbL). The nanoparticulate system was studied by scanning electron microscopy, steady-state, and their biological activity was evaluated using in vitro cancer cell lines by classical MTT assay. Results: The polyelectrolytic PLGA nanoparticles had an average diameter of 384.7 ± 138.6 nm, restricted distribution size with a polydispersity index. The obvious change in zeta potential indicates successful alternation in polycation (PAH) and polyanion (PSS) deposition directly in PLGA nanoparticles. Scanning electron microscopy (SEM) analysis showed that the formed system had morphology spherical, typical of these release systems. The loading efficiency was 82.1 % ± 1.2 %. The polyelectrolytic nanoparticles loaded with phthalocyanine maintained their photophysical behavior after encapsulation. Cell viability was determined, obtaining 90 % cell death. Conclusions: Therefore, the presented work depicts ZnPcSO4-loaded polyelectrolytic PLGA nanoparticles as a promise drug delivery system for phototherapeutic agent, which are thus expected to have superior therapeutic efficiency than free drug.
Development and characterization of ceramic-polymeric hybrid scaffolds for bone regeneration: incorporating of bioactive glass BG-58S into PDLLA matrix
(Taylor & Francis) Aguiar, Veronica Cristina Pêgo Fiebig; Bezerra, Rayssa do Nascimento; Santos, Kennedy Wallace dos; Gonçalves, Isabela dos Santos; Costa, Karen Julie Santos Grancianinov; Lauda, Diogo Ponte; Campos, Tiago Moreira Bastos; Prado, Renata Falchete do; Vasconcellos, Luana Marotta Reis de; Oliveira, Ivone Regina de
In recent years, there has been a notable surge of interest in hybrid materials within the biomedical field, particularly for applications in bone repair and regeneration. Ceramic-polymeric hybrid scaffolds have shown promising outcomes. This study aimed to synthesize bioactive glass (BG-58S) for integration into a bioresorbable poly- meric matrix based on PDLLA, aiming to create a bioactive scaffold featuring stable pH levels. The synthesis involved a thermally induced phase separation process followed by lyophilization to ensure an appropriate porous structure. BG-58S characterization revealed vitreous, bioactive, and mesoporous structural properties. The scaffolds were analyzed for morphology, interconnectivity, chemical groups, porosity and pore size distribution, zeta potential, pH, in vitro degradation, as well as cell viability tests, total protein content and mineralization nodule production. The PDLLA scaffold displayed a homogeneous morphology with interconnected mac- ropores, while the hybrid scaffold exhibited a heterogeneous mor- phology with smaller diameter pores due to BG-58S filling. The hybrid scaffold also demonstrated a pH buffering effect on the polymer surface. In addition to structural characteristics, degrada- tion tests indicated that by incorporating BG-58S modified the acidic degradation of the polymer, allowing for increased total pro- tein production and the formation of mineralization nodules, indi- cating a positive influence on cell culture.
Use of an inexpensive carbon source for the production of a cellulase enzyme complex from Penicillium ucsense S1M29 and enzymatic hydrolysis optimization
(Biofuels Bioproducts & Biorefining) Lima, Deise Juliana da Silva; Couto, Rafaela; Souza, Jucara Cristina Pereira; Camassola, Marli; Fontana, Roselei C.; Dillon, Aldo Jose; Pradella, Jose Geraldo da Cruz
The high cost of cellulolytic enzyme complexes (CECs) has been a significant impediment to the commercial production of bioproducts from lignocellulose biomass. This study aimed to develop a cost-effective CEC derived from Penicillium ucsense (former Penicillium echinulatum), utilizing diverse forms of pretreated sugarcane bagasse as the primary carbon/inductor source. Among the different pretreatments used, the hydrothermal pretreatment followed by NaOH delignification (BHD) produced higher FPase and xylanase activities (4.5 FPU mL–1 and 120 IU mL–1) in bioreactor experiments at 20 g BHD L–1 initial concentration. A batch-mode assay conducted across a range of initial carbon source (5 to 60 g L–1) confirmed the highest FPase activity (4.0 to 5.0 FPU mL–1 at 120 h), in the range of 20–40 g BHD L–1. During these assays the agitation rate, controlled by dissolved O2, tended to stabilize at lower levels, indicating substrate limitation. Conversely, higher initial carbon source concentrations led to an excess of glucose, likely triggering carbon catabolite repression and inhibiting cellulase production. This insight prompted the development of a controlled pulsed fed-batch strategy, resulting in FPase activity of 11 FPU mL–1 at 220 h using 90 g L–1 BHD controlled fed into the bioreactor. An enzymatic hydrolysis procedure using the generated CEC was also optimized using a central composite rotational design (CCRD). The optimized enzyme hydrolysis conditions achieved a reducing sugar concentration of 80.9 g L–1 in 48 h using 170 g L–1 of BHD as the substrate at a ratio of 15 FPU of enzyme substrate per g of BHD. A preliminary economic assessment demonstrated that, for a first- and second-generation (1G + 2G) ethanol biorefinery, the cost contribution of enzymes would be about US$0.2/L of biofuel. In conclusion, an efficient and highly productive procedure was developed successfully for the production of a CEC. It was particularly effective for the enzymatic hydrolysis of pretreated sugarcane bagasse.
Vaterite submicron particles designed for photodynamic therapy in cells
(Elsevier) Souza, Eliane de Fátima; Ambrósio, Jéssica Aparecida Ribeiro; Pinto, Bruna Cristina dos Santos; Beltrame Junior, Milton; Sakane, Kumiko Koibuchi; Pinto, Juliana Guerra; Ferreira-Strixino, Juliana; Gonçalves, Érika Peterson; Simioni, Andreza Ribeiro
Background: Calcium carbonate (CaCO3) is one of the most abundant materials in the world. It has several different crystalline phases as present in the minerals: calcite, aragonite and vaterite, which are anhydrous crystalline polymorphs. Regarding the preparation of these microparticles, the most important aspect is the control of the polymorphism, particle size and material morphology. This study aimed to develop porous microparticles of calcium carbonate in the vaterite phase for the encapsulation of chloro-aluminum phthalocyanine (ClAlPc) as a photosensitizer (PS) for application in Photodynamic Therapy (TFD). Methods: In this study, spherical vaterite composed of microparticles are synthesized by precipitation route assisted by polycarboxylate superplasticizer (PSS). The calcium carbonate was prepared by reacting a mixed solution of Na2CO3 with a CaCl2 solution at an ambient temperature, 25 °C, in the presence of polycarboxylate superplasticizer as a stabilizer. The photosensitizer was incorporated by adsorption technique in the CaCO3 microparticles. The CaCO3 microparticles were studied by scanning electron microscopy, steady-state, and their biological activity was evaluated using in vitro cancer cell lines by trypan blue exclusion method. The intracellular localization of ClAlPc was examined by confocal microscopy. Results: The CaCO3 microparticles obtained are uniform and homogeneously sized, non-aggregated, and highly porous microparticles. The calcium carbonate microparticles show an average size of 3 μm average pore size of about 30–40 nm. The phthalocyanine derivative loaded-microparticles maintained their photophysical behavior after encapsulation. The captured carriers have provided dye localization inside cells. The in vitro experiments with ClAlPc-loaded CaCO3 microparticles showed that the system is not cytotoxic in darkness, but exhibits a substantial phototoxicity at 3 μmol.L−1 of photosensitizer concentration and 10 J.cm-2 of light. These conditions are sufficient to kill about 80 % of the cells. Conclusions: All the performed physical–chemical, photophysical, and photobiological measurements indicated that the phthalocyanine-loaded CaCO3 microparticles are a promising drug delivery system for photodynamic therapy and photoprocesses.

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