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Bol. latinoam. Caribe plantas med. aromát ; 21(3): 389-403, mayo 2022. ilus, tab
Article in English | LILACS | ID: biblio-1397080


This study evaluated the specific interactions between drug and polymers in amorphous spray dried dispersions (SDDs). Four Biopharmaceutics Classification System (BCS) II class drugs were evaluated. Binary and ternary SDDs were manufactured with conventional polymers and arabinogalactan. Specific interaction parameters between drug and polymer were determined using theoretical calculations and DSC data. Analytical methods were used to evaluate solid and solution state interactions. Maximum amorphous content for each formulation was calculated using DSC. Flory-Huggins Specific Interaction Parameters were calculated. Negative specific parameters were associated with solid-state interactions and improved capacity of drug in the amorphous state. Ternary SDDs containing drug, polymer, and arabinogalactan displayed similar hydrogen bonding as was observed with binary SDDs. Solution-state interactions observed in binary systems may be used in tertiary systems to improve the amorphous drug capacity and improved dissolution compared to the binary. The resultant tertiary systems are an improvement over binary drug polymer systems.

Este estudio evaluó las interacciones específicas entre el fármaco y los polímeros en dispersiones amorfas secadas por pulverización (SDD). Se evaluaron cuatro fármacos de clase II del Sistema de Clasificación Biofarmacéutica (BCS). Los SDD binarios y ternarios se fabricaron con polímeros convencionales y arabinogalactano. Los parámetros de interacción específicos entre el fármaco y el polímero se determinaron utilizando cálculos teóricos y datos de DSC. Se utilizaron métodos analíticos para evaluar las interacciones del estado sólido y de la solución. El contenido amorfo máximo para cada formulación se calculó usando DSC. Se calcularon los parámetros de interacción específicos de Flory-Huggins. Los parámetros específicos negativos se asociaron con interacciones en estado sólido y una capacidad mejorada del fármaco en el estado amorfo. Los SDD ternarios que contienen fármaco, polímero y arabinogalactano mostraron enlaces de hidrógeno similares a los observados con los SDD binarios. Las interacciones de estado de solución observadas en sistemas binarios pueden usarse en sistemas terciarios para mejorar la capacidad del fármaco amorfo y mejorar la disolución en comparación con el binario. Los sistemas terciarios resultantes son una mejora con respecto a los sistemas de polímeros de fármacos binarios.

Polymers/chemistry , Solubility , Pharmaceutical Preparations/chemistry , Biological Availability , Temperature , X-Ray Diffraction , Microscopy, Electron, Scanning , Spectroscopy, Fourier Transform Infrared , Proton Magnetic Resonance Spectroscopy
Article in Chinese | WPRIM | ID: wpr-927916


The present study explored the effect of co-amorphous technology in improving the dissolution rate and stability of silybin based on the puerarin-silybin co-amorphous system prepared by the spray-drying method. Solid-state characterization was carried out by powder X-ray diffraction(PXRD), polarizing microscopy(PLM), Fourier transform infrared spectroscopy(FT-IR), differential scanning calorimetry(DSC), etc. Saturated powder dissolution, intrinsic dissolution rate, moisture absorption, and stability were further investigated. The results showed that puerarin and silybin formed a co-amorphous system at a single glass transition temperature which was higher than that of any crude drug. The intrinsic dissolution rate and supersaturated powder dissolution of silybin in the co-amorphous system were higher than those of the crude drug and amorphous system. The co-amorphous system kept stable for as long as three months under the condition of 40 ℃, 75% relative humidity, which was longer than that of the single amorphous silybin. Therefore, the co-amorphous technology could significantly improve the dissolution and stability of silybin.

Calorimetry, Differential Scanning , Desiccation , Drug Compounding/methods , Drug Stability , Silymarin , Solubility , Spectroscopy, Fourier Transform Infrared , Technology , X-Ray Diffraction
Braz. dent. sci ; 25(4): 1-10, 2022. tab, ilus, graf
Article in English | LILACS, BBO | ID: biblio-1395952


Objective: Endodontic perforation is a challenging mishap that should be repaired with a biocompatible material, Mineral trioxide aggregate (MTA) and Biodentine are the most commonly used repair materials. However, these materials are expensive, (MTA) has prolonged setting time and difficult manipulation. The purpose of this study is to prepare the experimental nano calcium-aluminate/tri-calcium-silicate (CA/C3S) material and comparing its physical properties with biodentine and MTA, to evaluate the experimental material eligibility to compete the commercial repair materials. And to perform part two (animal study) that will evaluate the cytotoxicity, the biocompatibility and the efficacy of (CA/C3S) in furcal perforation repair compared to diode laser. Material and Methods: A mixture of calcium carbonate and aluminum oxide was used to formulate calcium aluminate phase (CA), tri-calcium-Silicate phase (C3S) was formulated by firing of calcium carbonate and quartz. The produced powders were investigated by X-ray diffraction, then (CA) and (C3S) mixed with water.(CA/ C3S) compared with MTA and biodentine for setting-time, micro-hardness, dimensional-stability and solubility. Results: Mean setting time of (CA/C3S) was (32.70±0.75min) which is significantly higher than MTA and Biodentine. The Mean microhardness of (CA/C3S) was (56.50±7.41VHN) which has no statical difference with MTA and Biodentine. Solubility results showed weight increase for (CA/C3S) as following (6.29±3.05)and loss of weight for MTA and Biodentine. The percentage of change in dimensions for(CA/C3S) increased as following (0.64±0.78) while decreased for MTA and Biodentine. Conclusion: The experimental (CA/C3S) material showed good microhardness, dimensional stability and acceptable setting time that could be improved in further work (AU)

Objetivo: A perfuração endodôntica é um percalço desafiador que deve ser reparado com um material biocompatível, Agregado de trióxido mineral (MTA) e Biodentina são os materiais de reparo mais comumente usados. No entanto, esses materiais são caros, (MTA) tem tempo de presa prolongado e difícil manipulação. O objetivo deste estudo é preparar o material experimental de nano aluminato de cálcio/silicato tricálcico (CA/C3S) e comparar suas propriedades físicas com biodentina e MTA, para avaliar a elegibilidade do material experimental para competir com os materiais de reparo comerciais. E realizar a segunda parte (estudo animal) que avaliará a citotoxicidade, a biocompatibilidade e a eficácia do (CA/C3S) no reparo de perfuração de furca em comparação ao laser de diodo.Material e Métodos: Uma mistura de carbonato de cálcio e óxido de alumínio foi usada para formular a fase de aluminato de cálcio (CA), a fase tri-cálcio-silicato (C3S) foi formulada por queima de carbonato de cálcio e quartzo. Os pós produzidos foram investigados por difração de raios X, em seguida (CA) e (C3S) misturados com água. (CA/ C3S) comparados com MTA e biodentina para tempo de presa, microdureza, estabilidade dimensional e solubilidade. Resultados: O tempo médio de presa de (CA/C3S) foi (32,70±0,75min) que é significativamente maior que MTA e Biodentine. A microdureza média de (CA/C3S) foi (56,50±7,41VHN) que não tem diferença estática com MTA e Biodentine. Os resultados de solubilidade mostraram aumento de peso para (CA/C3S) conforme a seguir (6,29±3,05) e perda de peso para MTA e Biodentine. A porcentagem de mudança nas dimensões para (CA/C3S) aumentou como segue (0,64±0,78), enquanto diminuiu para MTA e Biodentine. Conclusão: O material experimental (CA/C3S) apresentou boa microdureza, estabilidade dimensional e aceitável tempo de presa, que pode ser melhorado em trabalhos futuros (AU)

X-Ray Diffraction , Biocompatible Materials , Calcium Carbonate , Lasers, Solid-State , Aluminum Oxide
Braz. J. Pharm. Sci. (Online) ; 58: e19519, 2022. tab, graf
Article in English | LILACS | ID: biblio-1383984


Abstract Silver nanoparticles (AgNPs) are among the most known nanomaterials being used for several purposes, including medical applications. In this study, Calendula officinalis L. flower extract and silver nitrate were used for green synthesis of silver nanoparticles under red, green and blue light-emitting diodes. AgNPs were characterized by Ultraviolet-Visible Spectrophotometry, Field Emission Scanning Electron Microscopy, Dynamic Light Scattering, Electrophoretic Mobility, Fourier Transform Infrared Spectroscopy and X-ray Diffraction. Isotropic and anisotropic silver nanoparticles were obtained, presenting hydrodinamic diameters ranging 90 - 180 nm, polydispersity (PdI > 0.2) and moderate stability (zeta potential values around - 20 mV)

Silver , Silver Nitrate/agonists , Calendula/adverse effects , Flowers/genetics , Nanoparticles/analysis , Spectrophotometry/methods , X-Ray Diffraction/methods , Microscopy, Electron, Scanning/methods , Spectroscopy, Fourier Transform Infrared , Light
Braz. J. Pharm. Sci. (Online) ; 58: e18946, 2022. tab, graf
Article in English | LILACS | ID: biblio-1364411


Abstract To investigate structure-property relationship of polymer-based curcumin solid dispersion (SD), three acrylic polymers were used to formulate curcumin SD by solvent evaporation method. Curcumin Eudragit EPO SD (cur@EPO), curcumin Eudragit RS PO SD (cur@RSPO) and curcumin Eudragit RL PO SD (cur@RLPO) showed deep red, golden orange and reddish orange color, respectively. Cur@RSPO entrapped 15.42 wt% of curcumin followed by cur@RL PO and cur@EPO. FTIR spectra indicated that in cur@EPO, curcumin may transfer hydrogen to the dimethylaminoethyl methacrylate group and thus change its color to red. In contrast, curcumin may form hydrogen bonding with Eudragit RS PO and Eudragit RL. Curcumin exists in amorphous state in three SDs as proved by differential scanning calorimetry and X-Ray diffraction measurement. In vitro digestion presented that lower pH value in simulated gastric fluid (SGF) stimulates the curcumin release from cur@EPO while permeability influences the release profile in other two SDs. When in simulated intestinal fluid (SIF), first order release model governs the release behaviors of all three SDs which showed sustained release pattern. Our results are helpful to elucidate how structure of polymer may impact on the major properties of curcumin contained SD and will be promising to broaden its therapeutic applications.

Polymers , Curcumin/analysis , Methods , Solvents/administration & dosage , X-Ray Diffraction/instrumentation , In Vitro Techniques/methods , Calorimetry, Differential Scanning/methods , Evaporation/classification , Spectroscopy, Fourier Transform Infrared , Color , Citrus sinensis/classification , Hydrogen-Ion Concentration
Bol. latinoam. Caribe plantas med. aromát ; 20(3): 226-243, may. 2021. ilus, tab
Article in English | LILACS | ID: biblio-1342815


Several species of the Myrcia genus have been used in folk medicine to treat diabetes. Therefore, the aim of this work was to investigate the inhibitory activity of α-glucosidase and pancreatic lipase in the crude extract (EBF) and in the ethyl acetate fraction (FFA) of Myrcia hatschbachii, as well as to identify isolated phenolic compounds and to evaluate the antioxidant property and preliminary in vitro toxicity against Artemia salina. EBF (IC50: 3.21 µg/mL) and FFA (IC50: 1.14 µg/mL) showed inhibitory activity superior to acarbose (IC50: 193.65 µg/mL). In addition, they showed inhibitory effects of pancreatic lipase (IC50: 556.58 µg/mL for EBF and 532.68 µg/mL for FFA), antioxidant potential, absence of preliminary toxicity and presence of gallic andellagic acids in FFA. The relevant results in the inhibition of α-glucosidase and pancreatic lipase motivate new studies for the development of herbal medicines that assist in the treatment of diabetic patients.

Varias especies del género Myrcia se han utilizado en la medicina popular para tratar la diabetes. Por lo tanto, el objetivo de este trabajo fue investigar la actividad inhibitoria de la α-glucosidasa y la lipasa pancreática en el extracto crudo (EBF) y en la fracción de acetato de etilo (FFA) de Myrcia hatschbachii, así como identificar compuestos fenólicos aislados y evaluar la propiedad antioxidante y toxicidad in vitro preliminar contra Artemia salina. EBF (IC50: 3.21 µg/mL) y FFA (IC50: 1.14 µg/mL) mostraron una actividad inhibitoria superior a la acarbosa (IC50: 193.65 µg/mL). Además, mostraron efectos inhibitorios de la lipasa pancreática (IC50: 556.58 µg/mL para EBF y 532.68 µg/mL para FFA), potencial antioxidante, ausencia de toxicidad preliminar y presencia de ácidos gálico y elágico en FFA. Los resultados relevantes en la inhibición de la α-glucosidasa y la lipasa pancreática motivan nuevos estudios para el desarrollo de medicamentos a base de hierbas que ayudan en el tratamiento de pacientes diabéticos.

Plant Extracts/pharmacology , Myrtaceae/chemistry , Glycoside Hydrolase Inhibitors/pharmacology , Lipase/drug effects , Antioxidants/pharmacology , Pancreas/enzymology , Phenols/analysis , X-Ray Diffraction , In Vitro Techniques , Plant Extracts/toxicity , Plant Extracts/chemistry , Free Radical Scavengers , Complex Mixtures , Ellagic Acid , Gallic Acid , Antioxidants/chemistry
São José dos Campos; s.n; 2021. 83 p. ilus, graf, tab.
Thesis in Portuguese | LILACS, BBO | ID: biblio-1362515


Os cimentos biocerâmicos possuem diversas aplicações clinicas na área de endodontia. Este estudo teve como objetivo avaliar a ação antimicrobiana do cimento de cinco óxidos minerais "5MO", do agregado trióxido mineral "MTA" que já é um material consagrado, como também do agregado trióxido mineral reparador de alta plasticidade "MTA HP", e comparar a capacidade dos mesmos na eliminação de microrganismos anaeróbios, comumente encontrados em infecções endodônticas primárias por meio de teste de MTT; avaliar e comparar também a biocompatibilidade dos mesmos através testes de citotoxicidade de MTT sobre cultura de macrófagos de camundongos (RAW 264.7) e osteoblastos (MG-63); avaliar a composição química dos mesmos através da microscopia eletrônica de varredura "MEV" acoplada a espectroscopia de raios X por dispersão em energia "EDS ou EDAX" e avaliar a fase por difração de raios-X "DRX"; além de avaliar a sua radiopacidade. Neste estudo, foi observada a atividade antibiofilme efetiva dos grupos experimentais sobre alguns microrganismos anaeróbios incluindo Porphyromonas gingivalis, Porphyromonas endodontalis, Parvimonas micra, Fusobacterium nucleatum e Prevotella intermedia, por outro lado, os mesmos foram biocompatíveis sobre os macrófagos e osteoblastos após 5 min de contato. Além disso, foram encontrados principais componentes químicos em que a presença de titânio, enxofre e potássio e a ausência de tungstênio no 5MO o torna diferente do MTA e do MTA HP, e a presença de estrôncio no MTA HP o torna diferente do 5MO e do MTA. Todos os biocerâmicos avaliados apresentaram uma radiopacidade adequada para serem utilizados clínicamente de acordo com o protocolo para radiopacidade de materiais dentários, publicado pela International Standards Organization (ISO). Sendo assim, os cimentos biocerâmicos 5MO, MTA HP, e MTA possuem ação antimicrobiana efetiva contra todos os microrganismos anaeróbios analisados, são biocompatíveis, possuem componentes químicos em comum, e possuem radiopacidade adequada para o uso clínico de material dentário.

Bioceramic cements have several clinical applications in endodontics. This study aimed to evaluate the antimicrobial action of the cement of five mineral oxides "5MO", mineral trioxide aggregate "MTA" which is already an established material, as well as the mineral trioxide aggregate repair high plasticity "MTA HP", and to compare their ability to eliminate anaerobic microorganisms, commonly found in primary endodontic infections by means of MTT test; to evaluate and compare their biocompatibility through MTT cytotoxicity tests on mouse macrophage cultures (RAW 264.7) and osteoblasts (MG-63); evaluate their chemical composition through scanning electron microscopy "SEM" coupled with energy dispersion X-ray spectroscopy "EDS or EDAX" and evaluate the phase by X-ray diffraction "XRD"; in addition to evaluating its radiopacity. In this study, all tested bioceramic cements were effective over some anaerobic microorganisms including Porphyromonas gingivalis, Porphyromonas endodontalis, Parvimonas micra, Fusobacterium nucleatum and Prevotella intermedia, on the other hand, they were biocompatible on macrophages and osteoblasts after 5 minutes of contact. In addition, main chemical components were found in which the presence of titanium, sulfur and potassium and the absence of tungsten in 5MO makes it different from MTA and MTA HP, and the presence of strontium in MTA HP makes it different from 5MO and MTA. All evaluated bioceramic cements presented adequate radiopacity to be used clinically according to the protocol for radiopacity of dental materials, published by the International Standards Organization (ISO). Thus, 5MO, MTA HP, and MTA bioceramic cements have effective antimicrobial action against all tested anaerobic microorganisms, are biocompatible, have chemical components in common, and have adequate radiopacity for the clinical use of dental material.

Animals , Mice , Biocompatible Materials , Dental Cements , Anti-Infective Agents , Anti-Bacterial Agents , X-Ray Diffraction , Microscopy, Electron, Scanning , Dental Materials
São José dos Campos; s.n; 2021. 70 p. ilus, tab, graf.
Thesis in Portuguese | LILACS, BBO | ID: biblio-1359883


O objetivo deste trabalho foi avaliar a resistência à fadiga e ciclos até a falha de 3 zircônias odontológicas após envelhecimento hidrotérmico isolado e um novo protocolo alternado. Discos de zircônia "Y"Z T (VITA), INCORIS "T"ZI (Dentsply Sirona) e "K"ATANA UTML (Noritake Kuraray) (N=135) ­ 1ª, 2ª e 3ª gerações, respectivamente ­, foram divididos em 9 grupos (n=15), com 3 tratamentos para cada zircônia: CF ­ Controle, somente com fadiga mecânica; EF ­ Envelhecido em reator hidrotérmico a 134 ºC por 20 h + Fadiga; EFA: 4 passos de envelhecimentos de 5h alternados com fadiga. O teste de fadiga em flexão biaxial foi realizado com configuração de pistão sob 3 esferas, utilizando o método step-stress (carga inicial: 100 Mpa, step: 50 MPa/10.000 ciclos, frequência: 20 Hz). Os dados foram analisados através de teste Kaplan-Meir e Mantel-Cox com α=0,05, além da análise de Weibull. Discos fraturados foram analisados em estereomicroscópio, Microscopia Eletrônica de Varredura (MEV) e Difratômetro de Raios-X (DRX). O envelhecimento isolado com fadiga aumentou a resistência do grupo TEF (810 ± 76 MPa), enquanto diminuiu a do YEF (516 ± 38 MPa), o protocolo alternado aumentou a resistência apenas para a YZ T (730 ± 59 MPa). A KATANA UMTL não apresentou diferenças para ambos os tratamentos. Igualmente, foi a única a não sofrer transformação de fase T-M. O grupo TEF apresentou maior taxa sobrevivência à fadiga (147,000.00 ciclos). A origem de fratura para todos os espécimes deu-se no lado de tração em defeitos pré-existentes. Zircônias de 2ª geração possuem melhor comportamento mecânico e longevidade pós-envelhecimento e fadiga. Embora seja menos resistente, a KATANA UTML não sofreu degradação

This study aimed to evaluate the fatigue strength and cycles for failure of 3 dental zirconias after isolated and a novel hydrothermal and mechanical fatigue cycling aging protocol. "Y"Z T (VITA), INCORIS "T"ZI (Dentsply Sirona) and "K"ATANA UTML (Noritake Kuraray) zirconia discs (N=135), were divided into 9 groups (n=15), according to 3 proposed treatments for each zirconia: CF (control ­ only mechanical fatigue cycling); AF (aging in hydrothermal reactor at 134°C for 20 h + mechanical fatigue cycling ); AFA (Alternating protocol: 4 steps of 5 h of hydrothermal aging intercalated with mechanical fatigue cycling). Mechanical fatigue aging was performed according to the step stress approach through biaxial flexural setup (piston-on-3-balls, initial strength: 100 MPa, step: 50 MPa/ci000, frequency: 20 Hz) until failure. Data were analyzed using KaplanMeier and Mantel-Cox test (α=0.05), in addition to Weibull analysis. Fractured discs were analyzed in stereomicroscope, Scanning Electron Microscopy and XRay Diffraction. Continuous hydrothermal and mechanical fatigue cycling decreased the fatigue strength of YAF group (516 ± 38 MPa), while the alternating protocol increased it (730 ± 59 MPa). KATANA UTML showed no differences for both treatments and did not undergo T-M phase transformation. The TAF group showed the highest fatigue strength (810 ± 76 MPa) and cycles for failure (147,000.00 cycles). The fracture origin for all specimens was on the tensile side in pre-existing defects. INCORIS TZI zirconia have higher fatigue strength after hydrothermal and mechanical fatigue aging. Although less resistant, KATANA UTML did not suffer chemical degradation

Tensile Strength , Zirconium/chemistry , Materials Testing , Ceramics , X-Ray Diffraction , Biocompatible Materials/analysis , Microscopy, Electrochemical, Scanning
Braz. dent. sci ; 24(2): 1-9, 2021. tab, ilus
Article in English | LILACS, BBO | ID: biblio-1177588


Objective: The purpose of the present study was to synthesize and characterize lithium disilicate glass-ceramics through the Li2O-SiO2system for determining the most satisfactory sintering parameter by evaluating the crystalline composition, microstructure and mechanical properties. Material and methods: The glass-ceramics were prepared from a glass precursor by means of the melting/cooling technique with a composition of 33.33 Li2O and 66.67 SiO2 (mol.%). The specimens were compressed by the uniaxial pressing technique and three different thermal treatments were used for sintering: 850 °C (Group 1), 900 °C (Group 2), and 950 °C (Group 3), which were determined based on the differential scanning calorimetry (DSC) result. The glass-ceramics were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Archimedes method, microhardness and biaxial flexural strength analyses. Results: The results regarding XRD predominantly showed lithium disilicate phase for all the heat treatments performed. Moreover, grains with a needle form were more predominantly observed in the SEM images for Group 3, as well as a higher densification and consequently higher mechanical properties. In contrast, Group 1 presented the lowest mechanical properties and densification, as well as the highest porosity. Conclusion: The present study demonstrated how extremely important it is to follow the heat treatment recommended by the manufacturers of ceramics, including time and temperature, which possess direct effects in the crystalline phase formation, as well as in the material's microstructure and mechanical properties (AU)

Objetivo: O presente estudo teve como objetivo sintetizar e caracterizar uma vitrocerâmica de dissilicato de lítio através do sistema Li2O-SiO2para determinar o parâmetro de sinterização mais satisfatório através da avaliação da composição cristalina, microestrutura e propriedades mecânicas. Material e Métodos: As vitrocerâmicas foram preparadas a partir de um vidro precursor pelo método fusão/resfriamento utilizando a composição de 33.33 Li2O e 66.67 SiO2 (mol.%). As amostras foram prensadas utilizando uma técnica de prensagem uniaxial e três tratamentos térmicos diferentes foram utilizadas para sinterização: 850 °C (Grupo 1), 900 °C (Grupo 2), e 950 °C (Grupo 3), que foram determinados através do resultado da análise diferencial de calorimetria. As vitrocerâmicas foram caracterizadas através das análises de difração de raios X (DRX), microscopia eletrônica de varredura (MEV), métodos de Arquimedes, microdureza e ensaio de flexão biaxial. Resultados: Os resultados de DRX mostraram predominantemente a fase de dissilicato de lítio para todos os tratamentos realizados. Além disso, grãos com forma agulhada foram mais predominantemente observados por MEV no grupo 3, assim como uma densificação maior e consequentemente valores maiores das propriedades mecânicas. Em contraste, o grupo 1 apresentou os menores valores de propriedades mecânicas e densificação, e também a maior porosidade. Conclusão: O presente estudo demonstrou como é extremamente importante seguir o tratamento térmico recomendado pelos fabricantes de cerâmica, incluindo tempo e temperatura, que possuem efeitos diretos na formação da fase cristalina, assim como na microestrutura do material e propriedades mecânicas. (AU)

X-Ray Diffraction , Microscopy, Electron, Scanning , Crystallization
Braz. dent. sci ; 24(3): 1-9, 2021. tab, ilus, graf
Article in English | LILACS, BBO | ID: biblio-1281728


Objective: The present study aimed to evaluate the effect of repressing and different surface treatment protocols on the shear bond strength of lithium disilicate glass-ceramics. Material and Methods: A total of 52 lithium disilicate glass-ceramic discs (IPS emax Press, Ivoclar Vivadent) were fabricated using the heat-press technique. The discs were divided into two groups; group (P): discs fabricated from new e.max ingots (n=26), group (R): discs fabricated from reused e.max buttons (n=26). Each group was subdivided into subgroup (E): discs were etched with hydrofluoric acid (9.5%) (n=13), subgroup (S): discs were air-abraded with 110 µm alumina particles. All specimens were subjected to X-ray Diffraction analysis, Scanning Electron Microscope, Energy Dispersive X-Ray, Thermo-Cycling, and Shear Bond Strength Testing. Results: Repressed Etched subgroup (RE) recorded the statistically highest shear bond strength value, followed by the Pressed Etched subgroup (PE), while the statistically lowest shear bond strength value was recorded for the Pressed Air-Abraded subgroup (PS) and Repressed Air-Abraded subgroup (RS). Conclusion: Repressing the leftover buttons for the construction of new lithium disilicate glass-ceramic restorations has no adverse effect on the bond strength of the resin cement to the ceramic. Hydrofluoric acid surface treatment improves the shear bond strength and durability of resin cement bond to both pressed and repressed lithium disilicate glass-ceramic. Air-abrasion cannot be considered as a reliable surface treatment when bonding to lithium disilicate glass-ceramics. (AU)

Objetivo: O presente estudo teve como objetivo avaliar o efeito da reprensagem e de diferentes protocolos de tratamento de superfície na resistência ao cisalhamento de vitrocerâmica de dissilicato de lítio. Materiais e Métodos: Um total de 52 discos de vitrocerâmica de dissilicato de lítio (IPS emax Press, Ivoclar Vivadent) foram fabricadas usando a técnica de prensagem quente. Os discos foram divididos em dois grupos: grupo (P): discos fabricados a partir de novo lingotes de e-max (n=26), grupo (R): discos fabricados a partir de botões de emax reutilizados (n=26). Cada grupo foi subdividido em subgrupo (E): discos condicionados com ácido fluorídrico (9,5%) (n=13), subgrupo (S) discos foram abrasivos com partícula 110 µm de alumínio. Todos os espécimes foram submetidos a analise de difração de raio-x, microscópio eletrônico de varredura, raio-x de energia dispersiva, termociclagem e teste de resistência de cisalhamento. Resultados: O subgrupo Reprensado-condicionado (RE) registrou o valor estatisticamente mais alta em relação a resistência ao cisalhamento, seguido pelo subgrupo Prensado-condicionado (PE), enquanto o valor estatisticamente mais baixo de resistência ao cisalhamento foi o subgrupo Prensado-Jateado (OS) e o subgrupo Reprensado-Jateado (RS). Conclusão: A reprensagem dos botões restantes para a construção de novas restaurações vitrocarâmicas de dissilicato de lítio não apresentou efeitos adversos na resistência de unicãp do cimento resinoso à cerâmica. O tratamento de superfície com ácido fluorídrico melhora a resistência ao cisalhamento e a durabilidade do cimento resinoso para vitrocerâmica de dissilicato de lítio prensada e reprimida. A abrasão por ar não pode ser considerada um tratamento de superfície confiável quanto a colagem da vitrocerâmica de dissilicato de lítio (AU)

X-Ray Diffraction , Resin Cements , Shear Strength , Microscopy, Electrochemical, Scanning
Article in English | WPRIM | ID: wpr-811435


PURPOSE: The aim of this study was to investigate the effect of different numbers of heat treatments applied to superstructure porcelain on optical, thermal, and phase formation properties of zirconia.MATERIALS AND METHODS: Forty zirconia specimens were prepared in the form of rectangular prism. Specimens were divided into four groups (n = 10) according to the number of firing at heating values of porcelain. Color differences and translucency parameter were measured, and X-ray diffraction (XRD) analysis and differential scanning calorimetry (DSC) were performed. Data were analyzed with analysis of variance (ANOVA).RESULTS: There were no statistically significant differences in ΔE, TP, L, a, and b value changes of the zirconia specimens as a result of repetitive firing processes (P>.05).CONCLUSION: Although additional firing processes up to 4 increase peak density in thermal analysis, additional firing processes up to 4 times can be applied safely as they do not result in a change in color and phase character of zircon frameworks.

Calorimetry, Differential Scanning , Dental Porcelain , Fires , Heating , Hot Temperature , X-Ray Diffraction
J. appl. oral sci ; 28: e20190371, 2020. tab, graf
Article in English | LILACS, BBO | ID: biblio-1056595


Abstract Objective This study aims to evaluate the influence of different air-abrasion pressures and subsequent heat treatment on the flexural strength, surface roughness, and crystallographic phases of highly translucent partially stabilized zirconia (Y-PSZ), and on the tensile bond strength of resin cement to Y-PSZ. Methodology Fully sintered zirconia specimens were ground with SiC paper (control) and/or air-abraded with 50 µm particles of alumina at 0.1, 0.15, 0.2, or 0.3 MPa or left as-sintered. After air-abrasion at 0.2 MPa (0.2AB), additional specimens were then heated to 1500°C, and held for one hour at this temperature (0.2AB+HT1h). Flexural strength and surface roughness were evaluated. Crystalline phase identification was also carried out using X-ray diffraction. Bonded zirconia specimens with self-adhesive resin cement were stored in distilled water at 37°C for 24 h, either with or without aging (thermal cycling 4-60°C/20000). Results were analyzed statistically by ANOVA and Tukey-Kramer tests. Results The flexural strength decreased with the increase in air-abrasion pressure, while in contrast, the surface roughness increased. The lowest flexural strength and the highest roughness value were found for the 0.2AB and 0.3AB groups, respectively. All groups contained cubic-, tetragonal ( t )-, and rhombohedral ( r )-ZrO2 phases with the exception of the as-sintered group. Upon increasing the air-abrasion pressure, the relative amount of the r -ZrO2 phase increased, with a significant amount of r -ZrO2 phase being detected for the 0.2AB and 0.3AB groups. The 0.2AB+HT1h group exhibited a similar flexural strength and t -ZrO2 phase content as the as-sintered group. However, the 0.2AB group showed a significantly higher tensile bond strength (p<0.05) than the 0.2AB+HT1h group before and after aging. Conclusion Micromechanical retention by alumina air-abrasion at 0.2 MPa, in combination with chemical bonding of a resin to highly translucent Y-PSZ using a MDP-containing resin cement may enable durable bonding.

Zirconium/chemistry , Dental Bonding/methods , Resin Cements/chemistry , Air Abrasion, Dental/methods , Aluminum Oxide/chemistry , Reference Values , Surface Properties , Tensile Strength , X-Ray Diffraction/methods , Materials Testing , Reproducibility of Results , Analysis of Variance , Microscopy, Confocal/methods , Flexural Strength , Hot Temperature
Braz. oral res. (Online) ; 34: e004, 2020. tab, graf
Article in English | LILACS | ID: biblio-1055523


Abstract The aim of this study was to analyze the structural, morphological and mechanical properties of two different lithium disilicate glass-reinforced ceramics for CAD-CAM systems (IPS e.max CAD and Rosetta SM). Five methodologies were used for both ceramics: microstructure (n = 2) was analyzed using x-ray diffraction (XRD); morphological properties (n = 2) were analyzed by scanning electron microscopy (SEM), with and without hydrofluoric etching; porosity (n = 3) was assessed using 3D micro-computed tomography (micro-CT); flexural strength was measured (n =1 0) using the three-point bending test; and bond strength was determined with self-adhesive resin cement (n = 10), using a microshear bond test. After performing all the tests, the data were analyzed using t-Student test and two-way ANOVA. All the tests used a significance level of α = 0.05. High peak positions corresponding to standard lithium metasilicate and lithium disilicate with similar intensities were observed for both ceramics in the XRD analysis. Morphological analysis showed that the crystalline structure of the two ceramics studied showed no statistical difference after acid etching. Additionally, no significant differences were recorded in the number or size of the pores for the ceramics evaluated. Moreover, no differences in flexural strength were found for the ceramic materials tested, or in the bond strength to ceramic substrates for the resin cements. Based on the study results, no significant differences were found between the two CAD-CAM lithium disilicate glass-reinforced ceramics tested, since they presented similar crystalline structures with comparable intensities, and similar total porosity, flexural strength and bond strength.

Ceramics/chemistry , Computer-Aided Design , Dental Porcelain/chemistry , Glass/chemistry , Reference Values , Surface Properties , X-Ray Diffraction , Materials Testing , Microscopy, Electron, Scanning , Reproducibility of Results , Analysis of Variance , Porosity , Dental Bonding/methods , Resin Cements/chemistry , Shear Strength , Flexural Strength
Braz. dent. j ; 30(5): 453-458, Sept.-Oct. 2019. graf
Article in English | LILACS | ID: biblio-1039141


Abstract The aim of this study was to analyze the effects of MTA on the structure and enzymatic activity of sPLA2 in order to provide subsidies for improvement in the formulation of the product. MTA powder was incubated for 60 min in the presence of sPLA2 and was analyzed by chromatography, electrospray mass (ESI-MS) and small-angle X-ray scattering (SAXS). It was find that the elution profile, retention time, and fragmentation of sPLA2 were altered after treatment with MTA. Calcium was the MTA component that most amplified the inflammatory signal. Significant interactions were found between MTA and sPLA2, which could aid in our understanding of the mechanisms of action of MTA during the inflammatory process and it may facilitate the structural modification of MTA, thereby improving its biological safety and consequently the rate of the treatment success.

Resumo O objetivo deste estudo foi analisar os efeitos do MTA na estrutura e atividade enzimática da sPLA2 a fim de fornecer subsídios para melhoria na formulação do produto. O MTA em pó foi incubado por 60 min na presença de sPLA2 e analisado por cromatografia, espectroscopia de massa por eletropulverização (ESI-MS) e espalhamento de raios-X de baixo ângulo (SAXS). Encontrou-se que o perfil de eluição, o tempo de retenção e a fragmentação da sPLA2 foram alterados após o tratamento com MTA. O cálcio foi o componente do MTA que mais ampliou o sinal inflamatório. Encontraram-se interações significativas entre o MTA e o sPLA2, o que poderia auxiliar na compreensão dos mecanismos de ação do MTA durante o processo inflamatório e facilitar a modificação estrutural do MTA, melhorando sua segurança biológica e consequentemente a taxa de sucesso do tratamento.

Root Canal Filling Materials , Oxides , X-Ray Diffraction , Silicates , Calcium Compounds , Aluminum Compounds , Drug Combinations , Scattering, Small Angle
Rev. biol. trop ; 67(1): 83-93, Jan.-Mar. 2019. tab, graf
Article in English | LILACS | ID: biblio-1041896


Abstract The solubility equilibrium of calcite is influenced by physicochemical, climatic and biological factors. Annual cycles of exceptionally prolonged drought, in conjunction with naturally occurring diffuse organic pollution, generate the unique conditions for the precipitation of lithified carbonate structures (microbialites). The aim of this article is to analyze the possible implications of calcite precipitation produced in mats of Cladophora sp. in an Andean subtropical basin, considering it is the first time this phenomenon is described for the region. We collected samples from selected sites at the Lules River Basin, in four sampling dates between the years 2003 and 2004, within a monitoring work of 15 years. Samples were analyzed using an electron microscope and X-ray diffraction analysis. We found that Gomphonema sp. attached to Cladophora sp. contributes to precipitation of calcite and formation of microbialite like structures, in the studied area. This work presents an initial discussion of the discovery of microbialites-like structures attached to Cladophora sp. mats in a subtropical Andean stream and the environmental conditions that lead to their production, as well as the possible ecological implications of these microbialites.(AU)

Resumen La fase sólida de las sales de los cuerpos de agua juega un papel importante en la concentración de los elementos mayoritarios. El equilibrio de solubilidad de la calcita está influenciado por factores fisicoquímicos, climáticos y biológicos. Los ciclos anuales de sequía excepcionalmente prolongada, junto con la contaminación orgánica difusa de origen natural, generan condiciones únicas para la precipitación de estructuras de carbonato litificado (microbialitos). El objetivo de este artículo es analizar las posibles implicaciones de la precipitación de calcita producida en Cladophora sp. en una cuenca subtropical andina, considerando que es la primera vez que se describe este fenómeno para la región. Recolectamos muestras en sitios seleccionados en la Cuenca del Río Lules, en cuatro fechas de muestreo entre 2003 y 2004, en el marco de un trabajo de monitoreo de quince años. Usamos red Surber para realizar los muestreos. Las muestras de algas, una vez libres de macroinvertebrados, se secaron y pesaron. Analizamos utilizando microscopía electrónica y difracción de rayos X. Encontramos que Gomphonema sp. unido a Cladophora contribuye a la precipitación de calcita y la formación de estructuras similares a microbialitos, en el área estudiada. Este trabajo presenta una discusión inicial sobre el descubrimiento de estructuras similares a microbialitos unidas a filamentos de Cladophora sp. en una cuenca andina subtropical y las condiciones ambientales que conducen a su producción, así como las posibles implicaciones ecológicas de lo mencionado anteriormente.(AU)

Lithium Carbonate/analysis , Diatoms/chemistry , Environmental Pollution , Droughts , Argentina , X-Ray Diffraction/instrumentation , Microscopy, Electron/instrumentation , Sampling Studies
J. appl. oral sci ; 27: e20180247, 2019. tab, graf
Article in English | LILACS, BBO | ID: biblio-975879


Abstract Objective This study aimed to investigate the effects of dodecacalcium hepta-aluminate (C12A7) content on some physicochemical properties and cytocompatibility of tricalcium silicate (C3S) cement using human dental pulp cells (hDPCs). Material and Methods High purity C3S cement was manufactured by a solid phase method. C12A7 was mixed with the cement in proportions of 0, 5, 8, and 10 wt% (C12A7-0, −5, −8, and −10, respectively). Physicochemical properties including initial setting time, compressive strength, and alkalinity were evaluated. Cytocompatibility was assessed with cell viability tests and cell number counts. Statistical analysis was performed by using one-way analysis of variance (ANOVA) and Tukey's test (p<0.05). Results The initial setting time of C3S-based cement was shorter in the presence of C12A7 (p<0.05). After 1 day, C12A7-5 showed significantly higher compressive strength than the other groups (p<0.05). After 7 days, the compressive strength of C12A7-5 was similar to that of C12A7-0, whereas other groups showed strength lower than C12A7-0. The pH values of all tested groups showed no significant differences after 1 day (p>0.05). The C12A7-5 group showed similar cell viability to the C12A7-0 group (p>0.05), while the other experimental groups showed lower values compared to C12A7-0 group (p<0.05). The number of cells grown on the C12A7-5 specimen was higher than that on C12A7-8 and −10 (p<0.05). Conclusions The addition of C12A7 to C3S cement at a proportion of 5% resulted in rapid initial setting time and higher compressive strength with no adverse effects on cytocompatibility.

Humans , Silicates/chemistry , Calcium Compounds/chemistry , Aluminum Compounds/chemistry , Dental Cements/chemistry , Dental Pulp Cavity/cytology , Particle Size , Reference Values , Time Factors , X-Ray Diffraction , Biocompatible Materials/pharmacology , Biocompatible Materials/chemistry , Materials Testing , Microscopy, Electron, Scanning , Cell Survival/drug effects , Cells, Cultured , Reproducibility of Results , Silicates/pharmacology , Calcium Compounds/pharmacology , Aluminum Compounds/pharmacology , Compressive Strength , Dental Cements/pharmacology , Dental Pulp Cavity/drug effects
Braz. arch. biol. technol ; 62: e19180266, 2019. tab, graf
Article in English | LILACS | ID: biblio-1055379


Abstract Phytochemical content of plant extracts can be used effectively to reduce the metal ions to nanoparticles in one-step green synthesis process. In this study, six plant extracts were used for the synthesis of silver nanoparticles (AgNPs). Biologically synthesized AgNPs was characterized using UV-Vis Spectrophotometer, Field Emission Scanning Electron Microscope (FE-SEM), X-ray diffraction (XRD), Energy Dispersive X-ray spectroscopy (EDX) and Fourier Transform Infrared (FTIR) spectroscopy. The individual and combined effects of AgNPs and tetracycline against S. aureus and K. pneumoniae were assessed. Ginger, onion and sidr extracts supported AgNPs formation while arak, garlic and mint extracts failed to convert the silver ions to AgNPs. The present findings revealed significant differences between the tested plant extracts in supporting AgNPs synthesis. AgNPs synthesized by ginger showed the highest individual and combined activity against tested strains followed by AgNPs prepared by sidr then that synthesized by onion. AgNPs significantly enhanced tetracycline activity (p≤0.05) against S. aureus and K. pneumoniae. The results of this study demonstrated that the combination of tetracycline and biologically synthesized AgNPs presented a useful therapeutically method for the treatment of bacterial infection and counterattacking bacterial resistance.

Silver/pharmacology , Staphylococcus aureus/drug effects , Tetracycline/biosynthesis , Plant Extracts/biosynthesis , Klebsiella pneumoniae/drug effects , Spectrometry, X-Ray Emission/instrumentation , X-Ray Diffraction/instrumentation , Spectrophotometers/methods , Spectroscopy, Fourier Transform Infrared/instrumentation
Article in Chinese | WPRIM | ID: wpr-777475


The powder X-ray diffraction(PXRD) technique was used to investigate fourteen kinds of Ranunculaceae herbal decoction pieces(RHDP) recorded in Chinese Pharmacopoeia and to explore a novel PXRD quality control method for RHDP. The results indicated that only three RHDP-Paeoniae Radix Alba, Paeoniae Radix Rubra, and Moutan Cortex, contained calcium oxalate monodydrate(COM), whereas no COM existed in other eleven kinds of RHDP. The difference in PXRD for Paeoniae Radix Alba and Paeoniae Radix Rubra from different growing areas were investigated. The quantitative analysis method for COM was discussed by considering the water-boiling manufacturing process of herbal decoction pieces. The water-boiling experiments revealed that the PXRD peaks from COM crystals in RHDP were enhanced significantly after boiling. Paeoniae Radix Alba, Paeoniae Radix Rubra, Moutan Cortex, Aconiti Lateralis Radix Praeparata, Aconiti Radix, Aconiti Kusnezoffii Radix, and Anemone Raddeanae Rhizoma exhibited a similar series of broader peaks in the 2θ region of 15° to 35°, whose origins were discussed on the basis of chemical constituents RHDP reported by other researchers. These diffraction broader peaks most likely originated from periodic orientation of benzene ring in organic molecular crystals of aconitine-and paeonolum-based alkaloids and glycosides chemical constituents, subsequently, possibly from some other organic constituents. The PXRD technique can be used to rapidly identify Cimicifuga heracleifolia with an amorphous dispersion peak and C. dahurica with a sharp-peak feature. Climatidis Radix et Rhizoma exhibited a series of sharp PXRD peaks. The PXRD method can provide a valuable quality control method for RHDP.

Aconitum , Chemistry , Drugs, Chinese Herbal , Chemistry , Paeonia , Chemistry , Phytochemicals , Ranunculaceae , Chemistry , Rhizome , Chemistry , X-Ray Diffraction
Article in English | WPRIM | ID: wpr-764043


In the present study, rutile phase titanium dioxide nanoparticles (R-TiO₂ NPs) were prepared by hydrolysis of titanium tetrachloride in an aqueous solution followed by calcination at 900℃. The composition of R-TiO₂ NPs was determined by the analysis of X-ray diffraction data, and the characteristic features of R-TiO₂ NPs such as the surface functional group, particle size, shape, surface topography, and morphological behavior were analyzed by Fourier-transform infrared spectroscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, transmission electron microscopy, dynamic light scattering, and zeta potential measurements. The average size of the prepared R-TiO₂ NPs was 76 nm, the surface area was 19 m²/g, zeta potential was −20.8 mV, and average hydrodynamic diameter in dimethyl sulfoxide (DMSO)–H₂O solution was 550 nm. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay and morphological observations revealed that R-TiO₂ NPs were cytocompatible with oral cancer cells, with no inhibition of cell growth and proliferation. This suggests the efficacy of R-TiO₂ NPs for the aesthetic white pigmentation of teeth.

Dimethyl Sulfoxide , Dynamic Light Scattering , Hydrodynamics , Hydrolysis , Microscopy, Electron, Scanning , Microscopy, Electron, Transmission , Mouth Neoplasms , Nanoparticles , Particle Size , Pigmentation , Spectrometry, X-Ray Emission , Spectrum Analysis , Titanium , Tooth , X-Ray Diffraction
Article in English | WPRIM | ID: wpr-742083


PURPOSE: The purpose of this study was to evaluate the effects of various protocols and systems for finishing and polishing monolithic zirconia on surface topography, phase transformation, and bacterial adhesion. MATERIALS AND METHODS: Three hundred monolithic zirconia specimens were fabricated and then treated with three finishing and polishing systems (Jota [JO], Meisinger [ME], and Edenta [ED]) using four surface treatment protocols: coarse finishing alone (C); coarse finishing and medium polishing (CM); coarse finishing and fine polishing (CF); and coarse finishing, medium polishing, and fine polishing (CMF). Surface roughness, crystal phase transformation, and bacterial adhesion were evaluated using atomic force microscopy, X-ray diffraction, and streptococcal biofilm formation assay, respectively. One-way and two-way analysis of variance with Tukey post hoc tests were used to analyze the results (α=.05). RESULTS: In this study, the surface treatment protocols and systems had significant effects on the resulting roughness. The CMF protocol produced the lowest roughness values, followed by CM and CF. Use of the JO system produced the lowest roughness values and the smallest biofilm mass, while the ME system produced the smallest partial transformation ratio. The ED group exhibited the highest roughness values, biofilm mass, and partial transformation ratio. CONCLUSION: Stepwise surface treatment of monolithic zirconia, combined with careful polishing system selection, is essential to obtaining optimal microstructural and biological surface results.

Bacterial Adhesion , Biofilms , Clinical Protocols , Dental Polishing , Microscopy, Atomic Force , X-Ray Diffraction