RESUMEN
The purification of flavonoids using the macroporous polymer resin method has gained attention in recent years due to its simplicity, precision, cost-effectiveness, and the ability to separate flavonoids from other constituents. Several studies have been conducted to investigate the efficiency and effectiveness of macroporous polymer resin in purifying flavonoids from various plant sources. This review aims to evaluate the existing literature on macroporous polymer resin purification of flavonoids and provide a comprehensive analysis of the current research trends and advancements in this field. It also highlights the importance of optimizing the adsorption parameters and conditions such as resin type, resin concentration, pH, and temperature for efficient purification of flavonoids using macroporous polymer resin. The key findings of this review reveal that macroporous resins with weak polarity, large surface areas, and pore diameters have a stronger adsorption capacity for flavonoids compared to polar resins. Furthermore, ultrasonic-solvent assisted extraction often combines with macroporous resin for effective the extraction and purification of flavonoids.
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Flavonoides , Plantas Medicinales , Polímeros , Resinas Sintéticas , Flavonoides/aislamiento & purificación , Flavonoides/química , Polímeros/química , Porosidad , Plantas Medicinales/química , Resinas Sintéticas/química , Adsorción , Propiedades de SuperficieRESUMEN
In this study, high-performance liquid chromatography was used to determine four components of Shaoyao Gancao Decoction (SGD), and the effect of purification was evaluated using fingerprints, similarity analysis and cell experiments. An effective method for isolation and purification of SGD was established. The adsorption/desorption properties of SGD were evaluated using resin screening, isothermal analysis, adsorption kinetics, and dynamic adsorption-desorption experiments. It was shown that the Langmuir equation fitted the isotherm data well and that a pseudo-second-order model accurately described kinetic adsorption on AB-8 resin. Analysis of thermodynamic parameters showed that the adsorption process was exothermic. Under the optimal process conditions, the concentrations of albiflorin, paeoniflorin, liquiritin and ammonium glycyrrhizinate in the product were 73.05, 134.04, 45.04 and 75.00 mg/g, respectively. The yields of the four components were 71.89 %-86.19 %. Cell experiments showed that the purified SGD retained anti-inflammatory activity. This research lays the foundation for the separation and purification of SGD and subsequent preparation research.
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Medicamentos Herbarios Chinos , Glucósidos , Monoterpenos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/aislamiento & purificación , Cromatografía Líquida de Alta Presión/métodos , Glucósidos/aislamiento & purificación , Glucósidos/química , Monoterpenos/aislamiento & purificación , Monoterpenos/química , Adsorción , Flavanonas/aislamiento & purificación , Flavanonas/química , Flavanonas/análisis , Animales , Ácido Glicirrínico/aislamiento & purificación , Ácido Glicirrínico/química , Ácido Glicirrínico/análisis , Hidrocarburos Aromáticos con Puentes/química , Hidrocarburos Aromáticos con Puentes/aislamiento & purificación , Ratones , Resinas Sintéticas/química , Antiinflamatorios/aislamiento & purificación , Antiinflamatorios/química , Humanos , Células RAW 264.7RESUMEN
An extraction chromatography resin, prepared by the impregnation of bis-octyloxy-calix[4]arene-mono-crown-6 (BOCMC)onto an acrylic ester based polymeric support material, gave excellent uptake data for the removal of radio-cesium (Cs-137) from nitric acid feed solutions. The weight distribution coefficient (Kd) value of >300 obtained during the present study at 3 M HNO3 was the highest reported so far while using a calix-crown-6 based extraction chromatographic resin material. Analogous resin reported previously has yielded a Kd value <100 at comparable feed conditions. The sorbed metal ions could be efficiently desorbed with de-ionized water. Kinetic modeling of the uptake data indicated that both the film and the intra-particle diffusion mechanism are simultaneously operating in the sorption of Cs+ion onto the BOCMC resin. The metal ion sorption data were fitted to the sorption isotherm models and did not conform to the chemisorptions of physisorption models and indicated a pi-pi interaction between the benzene rings of the calix-crown-6 ligand and the Cs+ ion. The reusability of the resins was quite satisfactory after 5 cycles and the radiation stability of the resin material was very good upto an absorbed dose of 500 kGy. The results of column studies were quite encouraging with 15 mL (9 bed volumes) as the breakthrough volume while the elution was complete in about 12 bed volumes of de-ionized water.
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Calixarenos , Calixarenos/química , Adsorción , Éteres Corona/química , Fenoles/química , Fenoles/aislamiento & purificación , Cinética , Resinas Sintéticas/química , Ligandos , Ácido Nítrico/químicaRESUMEN
The purpose of this work is to explore the properties of the lignin-derived amine-free photoinitiating systems (PISs) during the curing process. Four novel hydrogen donors (HD1, HD2, HD3, and HD4) derived from lignin α-O-4 structural were designed and synthesized by simple methods, and their low C-H bond dissociation energies on methylene were determined by molecular orbitals theory. Four experimental groups using CQ (camphorquinone)/HD PIs formulated with Bis-GMA/TEGDMA (70 w%/30 w%) were compared to CQ/EDB (ethyl 4-dimethylamino benzoate) system. The photopolymerization profiles and double bond conversion rate was tracked by FTIR experiments; the color bleaching ability of the samples and color aging test assay were performed using color indexes measurements; The cytotoxicity of the samples was also compared to EDB related systems. All of the experimental groups with new HDs were compared to the control group with EDB by statistical analysis. Compared to CQ/EDB system, new lignin-derived hydrogen donors combined with CQ showed comparable or even better performances in polymerization initiation to form resin samples, under a blue dental LED in air. Excellent color bleaching property was observed with the new HDs. Aging tests and cytotoxicity examination of the resin were performed, indicating the new lignin compounds to be efficient hydrogen donors for amine-free CQ-based photo-initiating system. Novel lignin α-O-4 derived hydrogen donors are promising for further usage in light-curing materials.
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Lignina , Polimerizacion , Lignina/química , Hidrógeno/química , Terpenos/química , Espectroscopía Infrarroja por Transformada de Fourier , Resinas Sintéticas/química , Materiales Dentales/química , Polietilenglicoles/química , Ácidos Polimetacrílicos/química , Alcanfor/análogos & derivadosRESUMEN
The study investigated the effects of temperature and centrifugation time on the efficacy of removing uncured resin from 3D-printed clear aligners. Using a photo-polymerizable polyurethane resin (Tera Harz TC-85, Graphy Inc., Seoul, Korea), aligners were printed and subjected to cleaning processes using isopropyl alcohol (IPA) or centrifugation (g-force 27.95g) at room temperature (RT, 23 °C) and high temperature (HT, 55 °C) for 2, 4, and 6 min. The control group received no treatment (NT). Cleaning efficiency was assessed through rheological analysis, weight measurement, transparency evaluation, SEM imaging, 3D geometry evaluation, stress relaxation, and cell viability tests. Results showed increased temperature and longer centrifugation times significantly reduced aligner viscosity, weight (P < 0.05), and transmittance. IPA-cleaned aligners exhibited significantly lower transparency and rougher surfaces in SEM images. All groups met ISO biocompatibility standards in cytotoxicity tests. The NT group had higher root mean square (RMS) values, indicating greater deviation from the original design. Stress relaxation tests revealed over 95% recovery in all groups after 60 min. The findings suggest that a 2-min HT centrifugation process effectively removes uncured resin without significantly impacting the aligners' physical and optical properties, making it a clinically viable option.
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Centrifugación , Impresión Tridimensional , Temperatura , Resinas Sintéticas/química , Poliuretanos/química , Supervivencia Celular/efectos de los fármacos , Ensayo de Materiales , Humanos , AnimalesRESUMEN
Atmospheric drying method for fabricating aerogels is considered the most promising way for casting aerogels on a large scale. However, the organic solvent exchange, remaining environmental pollution risk, is a crucial step in mitigating the impact of surface tension during the atmospheric drying process, especially for wet gel formed through the alkoxy-derived sol-gel process, such as melamine-formaldehyde resin (MF) aerogel. Herein, a tough polymer-assisted in situ polymerization was proposed to fabricate MF resin aerogel with a combination of mechanical toughness and strength, enabling it to withstand the capillary force during water evaporation. The monolithic MF resin aerogel through the sol-gel method can be directly prepared without additional network strengthening or organic solvent exchange. The resulting MF resin aerogel exhibits a homogeneous as well as hierarchical structure with macropores and mesopores (~6 µm and ~5 nm), high compressive modulus of 31.8 MPa, self-extinguishing property, and high-temperature thermal insulation with 97 % heat decrease for butane flame combustion. This work presents a straightforward and environmentally friendly method for fabricating MF resin aerogels with nanostructures and excellent performance in open conditions, exhibiting various applications.
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Retardadores de Llama , Geles , Triazinas , Triazinas/química , Geles/química , Presión , Solventes/química , Resinas Sintéticas/química , Desecación/métodos , Porosidad , PolimerizacionRESUMEN
The high energy density and robust cycle properties of lithium-ion batteries contribute to their extensive range of applications. Polyolefin separators are often used for the purpose of storing electrolytes, hence ensuring the efficient internal ion transport. Nevertheless, the electrochemical performance of lithium-ion batteries is constrained by its limited interaction with electrolytes and poor capacity for cation transport. This work presents the preparation of a new bio-based nanofiber separator by combining oxidized lignin (OL) and halloysite nanotubes (HNTs) with polyimide (PI) using an electrospinning technique. Analysis was conducted to examine and compare the structure, morphology, thermal characteristics, and EIS of the separator with those of commercially available polypropylene separator (PP). The results indicate that the PI@OL and PI-OL@ 10 % HNTs separators exhibit higher lithium ion transference number and ionic conductivity. Moreover, the use of HNTs successfully impeded the proliferation of lithium dendrites, hence exerting a beneficial impact on both the cycle performance and multiplier performance of the battery. Consequently, after undergoing 300 iterations, the battery capacity of LiFePO4|PI-OL@ 10 % HNTs|Li stays at 92.1 %, surpassing that of PP (86.8 %) and PI@OL (89.6 %). These findings indicate that this new bio-based battery separator (PI-OL@HNTs) has the great potential to serve as a substitute for the commonly used PP separator in lithium metal batteries.
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Arcilla , Suministros de Energía Eléctrica , Lignina , Litio , Nanofibras , Nanotubos , Litio/química , Nanotubos/química , Nanofibras/química , Lignina/química , Arcilla/química , Oxidación-Reducción , Resinas Sintéticas/químicaRESUMEN
The polyurethane (PU) foams can be functionally tailored by modifying the formulation with different additives. One such additive is melamine (MA) formaldehyde resin for improving their flame-retardant properties. In this work, the glycerol-modified (GMF), sodium alginate (SGMF)- and lignosulfonate-modified melamine formaldehyde (LGMF) were prepared and used as flame retardants reacting with isocyanate to prepare the corresponding rigid polyurethane foams (GMF-PU, SGMF-PU and LGMF-PU). The thermomechanical properties and flame-retardant properties of the foams were characterized. The results showed that the specific compression strength of GMF-PU, SGMF-PU and LGMF-PU increased substantially compared to the foams from physical addition of MA, sodium alginate and lignosulfonate, all of which were greater than that of the foam without any flame retardant (PPU). Meanwhile, the cell wall of the foam pores became thicker and the closed pore ratio increased. The sodium alginate and lignosulfonate played a key role in enhancing foam thermal stability. The limiting oxygen index values and cone calorimetry results indicated the flame-retardant efficiency of GMF-PU, SGMF-PU and LGMF-PU was significantly enhanced relative to PPU. Meanwhile, the heat and smoke release results indicated sodium alginate and lignosulfonate could reduce the amount of smoke generation to different degrees during the combustion of the foam.
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Alginatos , Retardadores de Llama , Lignina , Poliuretanos , Triazinas , Triazinas/química , Poliuretanos/química , Retardadores de Llama/análisis , Lignina/química , Lignina/análogos & derivados , Alginatos/química , Resinas Sintéticas/química , Glicerol/química , Temperatura , Formaldehído/química , Formaldehído/análisisRESUMEN
Phenolic resins occupy an important position in industrial applications, but phenol, one of the raw materials for synthesis, is a non-renewable resource. Lignin, as a natural polymer containing phenolic hydroxyl groups, alcohol hydroxyl groups and other reactive groups, can replace some of the phenol in the synthesis of phenolic resins, which can reduce the amount of phenol, thus reducing the cost of phenolic resins, while effectively promoting the high value-added use of renewable biomass resources. Due to its low reactivity, alkaline lignin is usually discharged as production waste, unaware that lignin macromolecules can be modified. In this paper, the phenolic monomers were obtained by acid-catalyzed depolymerization of DES (choline chloride/p-toluenesulfonic acid or choline chloride/lactic acid) from waste alkaline lignin, and the recovery rate of the DES solution during the catalytic treatment was more than 85 %, in which the main monomer was 2-methoxy-4-(1-propyl) phenol. The degradation of alkaline lignin is still favorable after five times of DES solvent recovery. The depolymerized lignin monomer replaced phenol by 50 wt% and then ternary co-polymerized with phenol and formaldehyde to form a biomass phenol-based phenolic resin, providing a green route for phenolic resin production. The cost of resin preparation was economically calculated, and it was found that the cost of resin after accumulating 4 cycles of DES treatment was only 51.1 % of that of pure phenolic resin. The density functional theory (DFT) was used to simulate the possible radical reactions in the intermediate process of phenolic resin reaction, to explore the microscopic mechanism and competition, to provide theoretical reference for further experimental realization of resin structure control and optimization, and to improve the theoretical system of resin synthesis.
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Lignina , Fenoles , Polimerizacion , Lignina/química , Fenoles/química , Catálisis , Fenol/química , Biomasa , Resinas Sintéticas/químicaRESUMEN
Silicon-containing arylacetylene resin and its composites have attracted great interest as emerging heat-resistant materials, but their curing mechanisms and products are still elusive. In this work, the influences of the terminal and inner acetylenes on the curing mechanisms of silicon-containing arylacetylene resin with 2,7-diethynylnaphthalene were first identified by density functional theory. Two reaction pathways were proposed and their products include polyenes, anthracene dimers, and benzene trimers. To gain a distinct observation of the cross-linking process, molecular dynamics simulations were used to construct a cross-linking polymerization model. The effects of the temperature on the cured structure were investigated by analyzing the characteristics of the cross-linked network. As expected, higher curing temperature will make the larger proportion of polyene chain and aromatic ring in the terminal alkyne-terminal alkyne route, meanwhile, for the inner alkyne-inner alkyne route, the short chains and a small amount of aromatic rings are major productions. Overall, our cross-linking method may provide an unique guidance for studying the cured structure of other thermosetting resins.
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Acetileno , Silicio , Silicio/química , Acetileno/química , Acetileno/análogos & derivados , Simulación de Dinámica Molecular , Naftalenos/química , Temperatura , Estructura Molecular , Reactivos de Enlaces Cruzados/química , Polimerizacion , Resinas Sintéticas/químicaRESUMEN
In this work, porous polyimide microfibers (PI-µF) were prepared by high-pressure wet spinning method, and successfully applied as adsorbents for solid phase extraction (SPE) of fluoroquinolones (FQs) in water and food samples. The PI-µFs of â¼10, 25, 50, 100 µm in diameter could be controlled by the inner diameter of quartz capillary nozzles. The flow resistance of SPE cartridges packed with 10 µm PI microfiber (10-PI-µF) and 25-PI-µF was comparable to or even lower than that of commercial SPE cartridges, while the flow resistance of 50-PI-µF and 100-PI-µF SPE cartridges was increased obviously due to tiny broken pieces. The 10-PI-µF and 25-PI-µF have a specific surface area of 102 m2 g-1 and 76 m2 g-1, mesopores of 22-32 nm, and large breakthrough volume of 110 mL/5 mg and 85 mL/5 mg for FQs, while the 50-PI-µF and 100-PI-µF had much lower specific surface area and hardly had retention for FQs. FQs from tap water, egg and milk samples were then extracted by PI-µF SPE, and analyzed by high performance liquid chromatography-fluorescence detector (HPLC-FLD). SPE parameters as type of elution solvent, elution solvent volume, pH value of sample solution, flow rate of sample solution, and breakthrough volume were first optimized in detail. Under the optimal conditions, the PI-µF SPE/HPLC-FLD method showed high recoveries (96.8%-107%), wide linearity (0.05-50 µg L-1, or 0.01-10 µg L-1), high determination coefficients (R2 ≥0.9992), and low limits of detection (LODs, 0.005-0.014 µg L-1). For the real tap water, egg and milk samples, the recoveries and RSDs were 81-119% and 0.8-9.8%, respectively. The results show that porous microfiber up to 25 µm in diameter is a promising solid-phase extraction adsorbent with the lowest flow resistance that can be used for trace organic pollutants in water and food samples.
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Fluoroquinolonas , Límite de Detección , Leche , Extracción en Fase Sólida , Contaminantes Químicos del Agua , Extracción en Fase Sólida/métodos , Fluoroquinolonas/análisis , Fluoroquinolonas/aislamiento & purificación , Fluoroquinolonas/química , Porosidad , Leche/química , Contaminantes Químicos del Agua/análisis , Contaminantes Químicos del Agua/aislamiento & purificación , Contaminantes Químicos del Agua/química , Cromatografía Líquida de Alta Presión/métodos , Animales , Huevos/análisis , Adsorción , Presión , Contaminación de Alimentos/análisis , Resinas Sintéticas/química , Análisis de los Alimentos/métodos , Reproducibilidad de los ResultadosRESUMEN
PURPOSE: The strength of temporary restorations plays a vital role in full-mouth reconstruction, and it can be impacted by the aging process. The aim of this in vitro study was to evaluate the biaxial flexural strength and fractographic features of different resin-based materials submitted to thermal aging. MATERIAL AND METHODS: One hundred and ninety-two resin disc-shaped specimens (6.5 mm in diameter and 0.5 mm in thickness) were fabricated and divided into six experimental groups according to the resin-based materials (Filtek Bulk-Fill flowable resin; J-Temp temporary resin; and Fuji Lining glass ionomer cement) and aging process (before and after thermal cycling). Biaxial flexural strength test was performed using a universal testing machine at a crosshead speed of 0.5 mm/min before and after thermal cycling (5 °C and 55 °C, 5760 cycles, 30 s). The mechanical properties were assessed using Weibull parameters (characteristic strength and Weibull modulus) (n = 30). Fractured specimens were examined under a polarized light stereomicroscope to identify crack origin and propagation direction. The surface microstructure of the resin-based materials was assessed by scanning electron microscopy (n = 2). The Weibull modulus (m), characteristic strength, and reliability properties were calculated, and a contour plot was used to detect differences among groups (95% confidence interval). RESULTS: The Weibull modulus (m), characteristic strength, and reliability of the resin-based compounds were influenced by material type and thermal aging (p < 0.05). Weibull modulus (m) revealed no differences when comparing the materials and aging process (p > 0.05), except for the preceding aging period where Filtek Bulk-Fill exhibited higher values compared to J-Temp (p < 0.05). Filtek Bulk-Fill demonstrated superior characteristic strength and reliability compared to J-Temp and Fuji Lining before and after thermal cycling (p < 0.05). Fractography of the resin-based materials showed fractures originating from surface defects exposed to tensile side and their propagation toward the compressive side. Generally, no differences in surface microstructure were observed on micrographs before and after thermal aging for Filtek Bulk-Fill and Fuji Lining. However, the aging process developed flaws in J-Temp. CONCLUSION: Resin-based material composition resulted in different flexural strength performance, impacting the Weibull modulus (m), characteristic strength, and reliability of the resin-based restorations.
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Resinas Compuestas , Resistencia Flexional , Ensayo de Materiales , Resinas Compuestas/química , Resinas Sintéticas/química , Temperatura , Factores de Tiempo , Agua/química , Estrés MecánicoRESUMEN
Post-detonation nuclear forensics capabilities depend on the ability to rapidly isolate radionuclides to improve measurement quality. In this work an extraction chromatography resin was developed utilizing thenoyltrifluoroacetone and 1-octanol supported on Eichrom prefilter resin. The resin was tested in nitric and hydrochloric acid matrices. In nitric acid the resin was able to extract zirconium, while in hydrochloric acid matrices it was possible to extract iron and gallium. In all acid conditions tested, gold was retained but can be eluted from the column with 10 % thiourea.
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Oro , Oro/química , Elementos de Series Actinoides/aislamiento & purificación , Elementos de Series Actinoides/química , Ácido Clorhídrico/química , Resinas Sintéticas/química , Circonio/química , Ácido Nítrico/químicaRESUMEN
This study aims to assess the efficacy of post-curing guidance supplied by 3D printing resin manufacturers. Current guidance applies generically to all geometries with the caveat that post-curing should be extended for 'large' or 'complex' geometries but specific guidance is not provided. Two vat-polymerisation 3D printers (Form3B, Figure 4 Standalone) were used to print test models in 6 biocompatible resins (Pro Black, Med White, Med Amber, Biomed Black, Biomed White, Biomed Amber). The test model is of a complex geometry whilst also housing ISO 527 test specimens in concentric layers. Two separate intervals of curing were applied (100%, 500% stated guidance) creating different curing treatments of the specimens throughout the model. Post processed test models were disassembled and pull testing performed on each of the specimens to assess the mechanical properties. The analysis showed that extending the curing duration had significant effects on the mechanical properties of some materials but not all. The layers of the model had a significant effect except for elongation at break for the Med Amber material. This research demonstrates that generic post-curing guidance regarding UV exposures is not sufficient to achieve homogenous material strength properties for complex geometries. Large variations in mechanical properties throughout the models suggest some material was not fully-cured. This raises a query if such materials as originally marketed as biocompatible are fully cured and therefore safe to use for medical applications involving complex geometries.
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Ensayo de Materiales , Fenómenos Mecánicos , Impresión Tridimensional , Materiales Biocompatibles/química , Factores de Tiempo , Pruebas Mecánicas , Resinas Sintéticas/químicaRESUMEN
The growing worry for human health stems from the fact that micropollutants (MPs), particularly dyes, are more common in aquatic settings. These particles pose a serious risk to both humans and animals since they have been found in a variety of bodily fluids and waste products from both humans and animals. MPs pose significant dangers to human health and other living things due to their extended half-lives, high fragmentation propensity, and capacity to absorb organic pollutants as well (MB, MR, MO and CV dyes) and heavy metals as well (Pb(II), Cd(II) Co(II) Cr(III) and Ag(I) .). They also contribute to the degradation of terrestrial and aquatic habitats. Sustainable and effective methods for removing MPs from wastewater and treating organic micropollutants in an environmentally friendly manner are being developed in order to address this problem. This work offers a thorough review of adsorption technology as a productive and environmentally friendly means of eliminating MPs from aqueous environments, with an emphasis on developments in the application of polymeric resin in MP removal. The review examines the adsorption process and the variables that affect adsorption efficiency, including the characteristics of the micropollutant, the resin, and the solution. To improve understanding, a number of adsorption mechanisms and models are explored. The study also addresses the difficulties and future possibilities of adsorption technology, emphasising the need to optimize resin characteristics, create sustainable and affordable regeneration techniques, and take into account the environmental effects of adsorbent materials.
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Restauración y Remediación Ambiental , Contaminantes Químicos del Agua , Adsorción , Contaminantes Químicos del Agua/química , Contaminantes Químicos del Agua/análisis , Restauración y Remediación Ambiental/métodos , Polímeros/química , Resinas Sintéticas/químicaRESUMEN
PURPOSE: To investigate the impact of printing layer thickness on the optical properties and surface roughness of various 3D-printed resins manufactured by digital light processing (DLP) and indicated for provisional and definitive restorations. MATERIALS AND METHODS: A total of 240 specimens from four different 3D-printing resins-VarseoSmile Crown Plus (Bego; VS), Crowntec (Saremco Dental; CR), GC Temp PRINT (GC Dental; TG), and NextDent C&B MFH (NextDent; ND)-were divided into four groups (n = 60 per group). Each group was further divided into three subgroups (n = 20) according to printing layer thickness (25, 50, and 100 µm). All specimens were subjected to thermocycling with coffee before measurements were taken with a spectroradiometer to calculate color differences. The Kubelka-Munk (K-M) absorption (K) and scattering coefficients (S), translucency parameters (TP), and surface roughness (Ra) values were calculated for each printing layer thickness and compared with those of the 2M2 shade tab (target). The data were analyzed using Mann-Whitney U test, the variance accounted for (VAF) coefficient by Cauchy-Schwarz, and post hoc comparisons using Tukey test (α ≤ .05). RESULTS: S (79% ≤ VAF ≤ 100%) and K (40.45% ≤ VAF ≤ 100%) spectral distribution depended on the wavelength. A 25-µm layer thickness resulted in no significant differences from the 2M2 shade for S (P > .230) and K (P > .200). VS showed significantly different S (P = .004) and K (P = .003) values from those of the shade tab with 50-µm layering thickness, whereas other materials did not show significant differences from the 2M2 shade for S (P > .280) and K (P > .301). The 100-µm layer thickness specimens had significantly different S and K values compared to the 2M2 shade tab (P < .004). TP values of resins with 100-µm layer thickness were significantly lower than resins in 25- and 50-µm layer thicknesses (P < .001). The Ra values of resins increased significantly with 100-µm layer thickness (P ≤ .001). CONCLUSIONS: All tested materials, except for VS, showed color properties similar to the target shade when 25- and 50-µm printing layer thicknesses were used. The translucency of resins tended toward an inverse relationship with printing layer thickness. The surface roughness of resins increased significantly with 100-µm layer thickness. However, all resins with a printing thickness of 25 µm showed better color properties and surface roughness.
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Impresión Tridimensional , Propiedades de Superficie , Ensayo de Materiales , Técnicas In Vitro , Resinas Compuestas/química , Resinas Sintéticas/químicaRESUMEN
In this study, a combination approach involving macroporous resin (MR) column chromatography and gradient countercurrent chromatography (CCC) was employed to enrich and purify bufadienolides from the roots and rhizomes of Helleborus thibetanus Franch. Initially, a D101 MR-packed column chromatography was utilized for fractionation and enrichment of the bufadienolides, which were effectively eluted from the column using a 60% ethanol solution. CCC was subsequently introduced to separate the enriched product using the ethyl acetate/n-butanol/water (EBuWat, 4:1:5, v/v) and EBuWat (5:0:5, v/v) solvent systems in a gradient elution mode. As results, five bufadienolides, including 6.1 mg of hellebrigenin-3-O-ß-D-glucoside (1), 2.2 mg of tigencaoside A (2), 8.3 mg of deglucohellebrin (3), 3.5 mg of 14 ß-hydroxy-3ß-[ß-D-glucopyranosyl-(1â6)-(ß-D-glucopyranosyl)oxy]-5α-bufa-20,22-dienolide (4), and 3.0 mg of 14ß-hydroxy-3ß-[(ß-D-glucopyranosyl)oxy]-5α-bufa-20,22-dienolide (5), were effectively separated from 300 mg of the enriched product. The respective high-performance liquid chromatography purities were as follows: 95.2%, 75.8%, 85.7%, 82.3%, and 92.8%. This study provides valuable insights for the efficient enrichment and separation of bufadienolides from Helleborus thibetanus Franch.
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Bufanólidos , Distribución en Contracorriente , Helleborus , Distribución en Contracorriente/métodos , Bufanólidos/química , Bufanólidos/aislamiento & purificación , Helleborus/química , Porosidad , Resinas Sintéticas/química , Cromatografía Líquida de Alta Presión , Raíces de Plantas/químicaRESUMEN
This preregistered ex vivo investigation examined the dentinal hybrid layer formation of a resinous infiltrant (Icon), with reference to both thickness (HLT) and homogeneity when combined with modified tunnel preparation (occlusal cavity only) and internal/external caries infiltration. The adhesives Syntac and Scotchbond MP were used as controls (Groups 1 and 3) or in combination with Icon (Groups 2 and 4). A split-tooth design using healthy third molars from 20 donors resulted in 20 prepared dentine cavities per experimental group. The cavity surfaces (n = 80) were etched (37% H3PO4), rinsed, and air-dried. Rewetting with ethanol was followed by application of the respective primers. After labeling with fluorescent dyes, either Syntac Adhesive/Heliobond or Scotchbond MP Adhesive was used alone or supplemented with Icon. HLT, as evaluated by scanning electron microscopy, did not significantly differ (P > 0.05), and confocal laser scanning microscopy revealed homogeneously mixed/polymerized resin-dentine interdiffusion zones in all groups. Icon can be successfully integrated into an ethanol-wet dentine bonding strategy, and will result in compact and homogeneous hybrid layers of comparable thickness considered equivalent to the non-Icon controls, thus allowing for preservation of the tooth's marginal ridge and interdental space in the case of internal/external infiltration of proximal caries.
Asunto(s)
Recubrimiento Dental Adhesivo , Esmalte Dental , Dentina , Etanol , Humanos , Etanol/química , Recubrimiento Dental Adhesivo/métodos , Recubrimientos Dentinarios/química , Tercer Molar , Cementos de Resina/química , Restauración Dental Permanente/métodos , Microscopía Confocal , Resinas Sintéticas/química , Caries Dental/terapia , Microscopía Electrónica de Rastreo , Resinas Compuestas/químicaRESUMEN
BACKGROUND: Three-dimensional (3D) printing is increasingly used to fabricate dental restorations due to its enhanced precision, consistency and time and cost-saving advantages. The properties of 3D-printed resin materials can be influenced by the chosen printing orientation which can impact the mechanical characteristics of the final products. PURPOSE: The objective of this study was to evaluate the influence of printing orientation and artificial ageing on the Martens hardness (HM) and indentation modulus (EIT) of 3D-printed definitive and temporary dental restorative resins. METHODS: Disk specimens (20 mm diameter × 2 mm height) were additively manufactured in three printing orientations (0°, 45°, 90°) using five 3D-printable resins: VarseoSmile Crownplus (VCP), Crowntec (CT), Nextdent C&B MFH (ND), Dima C&B temp (DT), and GC temp print (GC). The specimens were printed using a DLP 3D-printer (ASIGA MAX UV), while LavaTM Ultimate (LU) and Telio CAD (TC) served as milled control materials. Martens hardness (HM) and indentation modulus (EIT) were tested both before and after storage in distilled water and artificial saliva for 1, 30, and 90 days at 37 °C. RESULTS: 90° printed specimens exhibited higher HM than the other orientations at certain time points, but no significant differences were observed in HM and EIT between orientations for all 3D-printed materials after 90 days of ageing in both aging media. LU milled control material exhibited the highest HM and EIT among the tested materials, while TC, the other milled control, showed similar values to the 3D printed resins. CT and VCP (definitive resins) and ND displayed higher Martens parameters compared to DT and GC (temporary resins). The hardness of the 3D-printed materials was significantly impacted by artificial ageing compared to the controls, with ND having the least hardness reduction percentage amongst all 3D-printed materials. The hardness reduction percentage in distilled water and artificial saliva was similar for all materials except for TC, where higher reduction was noted in artificial saliva. SIGNIFICANCE: The used 3D printed resins cannot yet be considered viable alternatives to milled materials intended for definitive restorations but are preferable for use as temporary restorations.
Asunto(s)
Dureza , Ensayo de Materiales , Impresión Tridimensional , Módulo de Elasticidad , Materiales Dentales/química , Propiedades de Superficie , Resinas Compuestas/química , Factores de Tiempo , Restauración Dental Permanente , Resinas Sintéticas/químicaRESUMEN
OBJECTIVES: This in vitro pilot study aimed to evaluate whether different pre-treatments (demineralization, deproteinization, (chemo-)mechanical reduction of the surface layer) influence the penetration depth of a resin infiltrant into MIH-affected enamel compared to initial carious lesions. METHODS: Thirty extracted human permanent molars with non-cavitated initial carious lesions (n = 5) or MIH (n = 25) were chosen and randomly assigned to six experimental groups: IC: initial caries; M: MIH; MN: MIH, 5.25% sodium hypochlorite; MM: MIH, microabrasion; MA: MIH, air abrasion; MAN: MIH, air abrasion and 5.25% sodium hypochlorite. A modified indirect dual fluorescence staining method was adopted to assess the penetration depth (PD) of the resin infiltrant and the lesion depth (LD) by confocal laser scanning microscopy (CLSM). Exemplarily, scanning electron microscopic (SEM) images were captured. The relationship between group assignment and penetration/lesion depth was estimated using a linear mixed model incorporating the tooth as random effect (two observations/tooth). The significance level was set at p < 0.05. RESULTS: For MIH-affected molars, the mean PD (in µm; median, [minimum-maximum]) were M (178.2 [32.5-748.9]), MN (275.6 [105.3-1131.0]), MM (48.7 [0.0-334.4]), MA (287.7 [239.4-491.7]), and MAN (245.4 [76.1-313.5]). Despite the observed differences in PD between the groups, these could not be statistically verified (Bonferroni, p = 0.322). The percentage penetration was significantly higher for IC than for MIH groups (Bonferroni, p < 0.05). SIGNIFICANCE: Compared to IC, resin infiltration into MIH-affected enamel ist more variable. Different pre-treatments influence the resin penetration into developmentally hypomineralized enamel to a fluctuating level.