RESUMEN
Currently, there is no consensus in terms of defining the minimum radiant exposure values necessary for achieving adequate properties of composite resin. In addition, the long-term influence that radiant exposure has on the properties of composite resins is still questionable. OBJECTIVE: The objective of this study was to evaluate the effect of radiant exposure and UV accelerated aging on the physico-chemical and mechanical properties of micro-hybrid and nanofilled composite resins. MATERIAL AND METHODS: A nanofilled (Filtek Supreme; 3M ESPE) and a micro-hybrid composite resin (Filtek Z250; 3M ESPE) were investigated under different radiant exposures (3.75, 9, and 24 J/cm2) and UV accelerated aging protocols (0, 500, 1000, and 1500 aging hours). The degree of conversion (DC), flexural strength (FS), modulus (M), water sorption (WS), and solubility (WL) were evaluated. The results obtained were analyzed using two-way ANOVA and Tukey's test. Comparisons were performed using a significance level of α=0.05. RESULTS: The DC, FS, and M were found to be significantly influenced by both radiant exposure and accelerated aging time. The DC and EM increased with radiant exposure in the no-aging group (0-hour aging) for both micro-hybrid and nanofilled composites, whereas no correlation was found after accelerated aging protocols. WS and WL of micro-hybrid and nanofilled composite resins were scarcely affected by radiant exposure (p>0.05), whereas they were significantly reduced by accelerated aging (p<0.001). CONCLUSIONS: Although increasing radiant exposure affected the degree of conversion and mechanical properties of micro-hybrid and nanofilled composites, no influence on the hydrolytic degradation of the material was observed. In contrast, UV accelerated aging affected both the physico-chemical and mechanical properties of the composites.
Asunto(s)
Resinas Compuestas/química , Resinas Compuestas/efectos de la radiación , Rayos Ultravioleta , Análisis de Varianza , Luces de Curación Dental , Resistencia Flexional/efectos de la radiación , Ensayo de Materiales , Microscopía Electrónica de Rastreo , Transición de Fase/efectos de la radiación , Procesos Fotoquímicos/efectos de la radiación , Polimerizacion/efectos de la radiación , Dosis de Radiación , Valores de Referencia , Solubilidad , Espectroscopía Infrarroja por Transformada de Fourier , Propiedades de Superficie/efectos de la radiación , Factores de Tiempo , Agua/químicaRESUMEN
Abstract Currently, there is no consensus in terms of defining the minimum radiant exposure values necessary for achieving adequate properties of composite resin. In addition, the long-term influence that radiant exposure has on the properties of composite resins is still questionable. Objective: The objective of this study was to evaluate the effect of radiant exposure and UV accelerated aging on the physico-chemical and mechanical properties of micro-hybrid and nanofilled composite resins. Material and Methods: A nanofilled (Filtek Supreme; 3M ESPE) and a micro-hybrid composite resin (Filtek Z250; 3M ESPE) were investigated under different radiant exposures (3.75, 9, and 24 J/cm2) and UV accelerated aging protocols (0, 500, 1000, and 1500 aging hours). The degree of conversion (DC), flexural strength (FS), modulus (M), water sorption (WS), and solubility (WL) were evaluated. The results obtained were analyzed using two-way ANOVA and Tukey's test. Comparisons were performed using a significance level of α=0.05. Results: The DC, FS, and M were found to be significantly influenced by both radiant exposure and accelerated aging time. The DC and EM increased with radiant exposure in the no-aging group (0-hour aging) for both micro-hybrid and nanofilled composites, whereas no correlation was found after accelerated aging protocols. WS and WL of micro-hybrid and nanofilled composite resins were scarcely affected by radiant exposure (p>0.05), whereas they were significantly reduced by accelerated aging (p<0.001). Conclusions: Although increasing radiant exposure affected the degree of conversion and mechanical properties of micro-hybrid and nanofilled composites, no influence on the hydrolytic degradation of the material was observed. In contrast, UV accelerated aging affected both the physico-chemical and mechanical properties of the composites.
Asunto(s)
Rayos Ultravioleta , Resinas Compuestas/efectos de la radiación , Resinas Compuestas/química , Dosis de Radiación , Valores de Referencia , Solubilidad , Propiedades de Superficie/efectos de la radiación , Factores de Tiempo , Ensayo de Materiales , Agua/química , Microscopía Electrónica de Rastreo , Análisis de Varianza , Espectroscopía Infrarroja por Transformada de Fourier , Transición de Fase/efectos de la radiación , Luces de Curación Dental , Procesos Fotoquímicos/efectos de la radiación , Polimerizacion/efectos de los fármacos , Resistencia Flexional/efectos de la radiaciónRESUMEN
INTRODUCTION: High levels of shrinkage stress caused by volumetric variations during the activation process are one of the main problems in the practical application of composite resins. OBJECTIVE: The aim of this study is to reduce the shrinkage stress and minimize the effects caused by composite resin volumetric variation due to the photopolymerization. In this way, this work proposes a systematic study to determine the optimal dimming function to be applied to light curing processes. MATERIAL AND METHODS: The study was performed by applying mathematical techniques to the optimization of nonlinear objective functions. The effectiveness of the dimming function was evaluated by monitoring the polymerization shrinkage stress during the curing process of five brands/models of composites. This monitoring was performed on a universal testing machine using two steel bases coupled in the arms of the machine where the resin was inserted and polymerized. The quality of the composites cured by the proposed method was analyzed and compared with the conventional photoactivation method by experiments to determine their degree of conversion (DC). Absorbance measurements were performed using Fourier-transform infrared spectroscopy (FT-IR). A T-test was performed on DC results to compare the photoactivation techniques. We also used scanning electron microscopy (SEM) to analyze in-vitro the adhesion interface of the resin in human teeth. RESULTS: Our results showed that the use of the optimal dimming function, named as exponential, resulted in the significant reduction of the shrinkage stress (~36.88% ±6.56 when compared with the conventional method) without affecting the DC (t=0.86, p-value=0.44). The SEM analyses show that the proposed process can minimize or even eliminate adhesion failures between the tooth and the resin in dental restorations. CONCLUSION: The results from this study can promote the improvement of the composite resin light curing process by the minimization of polymerization shrinkage effects, given an operational standardization of the photoactivation process.
Asunto(s)
Resinas Compuestas/química , Resinas Compuestas/efectos de la radiación , Curación por Luz de Adhesivos Dentales/métodos , Polimerizacion/efectos de la radiación , Adhesividad , Análisis del Estrés Dental , Ensayo de Materiales , Microscopía Electrónica de Rastreo , Transición de Fase/efectos de la radiación , Valores de Referencia , Espectroscopía Infrarroja por Transformada de Fourier , Estrés Mecánico , Factores de TiempoRESUMEN
Abstract High levels of shrinkage stress caused by volumetric variations during the activation process are one of the main problems in the practical application of composite resins. Objective The aim of this study is to reduce the shrinkage stress and minimize the effects caused by composite resin volumetric variation due to the photopolymerization. In this way, this work proposes a systematic study to determine the optimal dimming function to be applied to light curing processes. Material and Methods The study was performed by applying mathematical techniques to the optimization of nonlinear objective functions. The effectiveness of the dimming function was evaluated by monitoring the polymerization shrinkage stress during the curing process of five brands/models of composites. This monitoring was performed on a universal testing machine using two steel bases coupled in the arms of the machine where the resin was inserted and polymerized. The quality of the composites cured by the proposed method was analyzed and compared with the conventional photoactivation method by experiments to determine their degree of conversion (DC). Absorbance measurements were performed using Fourier-transform infrared spectroscopy (FT-IR). A T-test was performed on DC results to compare the photoactivation techniques. We also used scanning electron microscopy (SEM) to analyze in-vitro the adhesion interface of the resin in human teeth. Results Our results showed that the use of the optimal dimming function, named as exponential, resulted in the significant reduction of the shrinkage stress (~36.88% ±6.56 when compared with the conventional method) without affecting the DC (t=0.86, p-value=0.44). The SEM analyses show that the proposed process can minimize or even eliminate adhesion failures between the tooth and the resin in dental restorations. Conclusion The results from this study can promote the improvement of the composite resin light curing process by the minimization of polymerization shrinkage effects, given an operational standardization of the photoactivation process.
Asunto(s)
Resinas Compuestas/efectos de la radiación , Resinas Compuestas/química , Curación por Luz de Adhesivos Dentales/métodos , Polimerizacion/efectos de la radiación , Valores de Referencia , Estrés Mecánico , Factores de Tiempo , Ensayo de Materiales , Microscopía Electrónica de Rastreo , Adhesividad , Espectroscopía Infrarroja por Transformada de Fourier , Análisis del Estrés Dental , Transición de Fase/efectos de la radiaciónRESUMEN
OBJECTIVE: This study aimed to investigate the effect of laser diode irradiation on the degree of conversion (DC), water sorption (WS), and water solubility (WSB) of these bonding systems in an attempt to improve their physico-mechanical resistance. MATERIAL AND METHODS: Two bonding agents were tested: a two-step total-etch system [Adper™ Single Bond 2, 3M ESPE (SB)] and a universal system [Adper™ Single Bond Universal, 3M ESPE (SU)]. Square-shaped specimens were prepared and assigned into 4 groups (n=5): SB and SU (control groups - no laser irradiation) and SB-L and SU-L [SB and SU laser (L) - irradiated groups]. DC was assessed using Fourier transform infrared spectroscopy with attenuated total reflectance. Additional uncured resin samples (≈3.0 µL, n=5) of each adhesive were also scanned for final DC calculation. For WS/WSB tests, similar specimens (n=10) were prepared and measured by monitoring the mass changes after dehydration/water storage cycles. For both tests, adhesive fluids were dropped into standardized Teflon molds (6.0×6.0×1.0 mm), irradiated with a 970-nm laser diode, and then polymerized with an LED-curing unit (1 W/cm2). RESULTS: Laser irradiation immediately before photopolymerization increased the DC (%) of the tested adhesives: SB-L>SB>SU-L>SU. For WS/WSB (µg/mm3), only the dentin bonding system (DBS) was a significant factor (p<0.05): SB>SU. CONCLUSION: Irradiation with a laser diode improved the degree of conversion of all tested simplified dentin bonding systems, with no impact on water sorption and solubility.
Asunto(s)
Recubrimientos Dentinarios/efectos de la radiación , Láseres de Semiconductores , Polimerizacion/efectos de la radiación , Luces de Curación Dental , Cementos Dentales/química , Cementos Dentales/efectos de la radiación , Recubrimientos Dentinarios/química , Curación por Luz de Adhesivos Dentales/métodos , Transición de Fase/efectos de la radiación , Procesos Fotoquímicos/efectos de la radiación , Valores de Referencia , Reproducibilidad de los Resultados , Solubilidad/efectos de la radiación , Espectroscopía Infrarroja por Transformada de Fourier , Estadísticas no Paramétricas , Propiedades de Superficie/efectos de la radiaciónRESUMEN
Abstract Simplified dentin-bonding systems are clinically employed for most adhesive procedures, and they are prone to hydrolytic degradation. Objective This study aimed to investigate the effect of laser diode irradiation on the degree of conversion (DC), water sorption (WS), and water solubility (WSB) of these bonding systems in an attempt to improve their physico-mechanical resistance. Material and Methods Two bonding agents were tested: a two-step total-etch system [Adper™ Single Bond 2, 3M ESPE (SB)] and a universal system [Adper™ Single Bond Universal, 3M ESPE (SU)]. Square-shaped specimens were prepared and assigned into 4 groups (n=5): SB and SU (control groups - no laser irradiation) and SB-L and SU-L [SB and SU laser (L) - irradiated groups]. DC was assessed using Fourier transform infrared spectroscopy with attenuated total reflectance. Additional uncured resin samples (≈3.0 µL, n=5) of each adhesive were also scanned for final DC calculation. For WS/WSB tests, similar specimens (n=10) were prepared and measured by monitoring the mass changes after dehydration/water storage cycles. For both tests, adhesive fluids were dropped into standardized Teflon molds (6.0×6.0×1.0 mm), irradiated with a 970-nm laser diode, and then polymerized with an LED-curing unit (1 W/cm2). Results Laser irradiation immediately before photopolymerization increased the DC (%) of the tested adhesives: SB-L>SB>SU-L>SU. For WS/WSB (μg/mm3), only the dentin bonding system (DBS) was a significant factor (p<0.05): SB>SU. Conclusion Irradiation with a laser diode improved the degree of conversion of all tested simplified dentin bonding systems, with no impact on water sorption and solubility.
Asunto(s)
Recubrimientos Dentinarios/efectos de la radiación , Láseres de Semiconductores , Polimerizacion/efectos de la radiación , Valores de Referencia , Solubilidad/efectos de la radiación , Propiedades de Superficie/efectos de la radiación , Reproducibilidad de los Resultados , Recubrimientos Dentinarios/química , Espectroscopía Infrarroja por Transformada de Fourier , Estadísticas no Paramétricas , Cementos Dentales/efectos de la radiación , Cementos Dentales/química , Transición de Fase/efectos de la radiación , Curación por Luz de Adhesivos Dentales/métodos , Luces de Curación Dental , Procesos Fotoquímicos/efectos de la radiaciónRESUMEN
Using giant unilamellar vesicles (GUVs) made from POPC, DPPC, cholesterol and a small amount of a porphyrin-based photosensitizer that we name PE-porph, we investigated the response of the lipid bilayer under visible light, focusing in the formation of domains during the lipid oxidation induced by singlet oxygen. This reactive species is generated by light excitation of PE-porf in the vicinity of the membrane, and thus promotes formation of hydroperoxides when unsaturated lipids and cholesterol are present. Using optical microscopy we determined the lipid compositions under which GUVs initially in the homogeneous phase displayed Lo-Ld phase separation following irradiation. Such an effect is attributed to the in situ formation of both hydroperoxized POPC and cholesterol. The boundary line separating homogeneous Lo phase and phase coexistence regions in the phase diagram is displaced vertically towards the higher cholesterol content in respect to ternary diagram of POPC:DPPC:cholesterol mixtures in the absence of oxidized species. Phase separated domains emerge from sub-micrometer initial sizes to evolve over hours into large Lo-Ld domains completely separated in the lipid membrane. This study provides not only a new tool to explore the kinetics of domain formation in mixtures of lipid membranes, but may also have implications in biological signaling of redox misbalance.
Asunto(s)
Luz , Peroxidación de Lípido/efectos de la radiación , Lípidos de la Membrana/química , Membranas Artificiales , Transición de Fase/efectos de la radiación , Procesos Fotoquímicos/efectos de la radiaciónRESUMEN
In the current study, the degree of conversion (DC) of bonding agents photoactivated using QTH or LED light-curing units (LCUs) was evaluated by Fourier Transform infrared spectroscopy with an attenuated total reflectance (ATR) device. Four LCUs were evaluated: one QTH (Optilux 501; Demetron Kerr) and three LEDs: Radii Cal (SDI), Elipar FreeLight 2 (3M ESPE) and Bluephase (Ivoclar Vivadent). Two etch-and-rinse (Scotchbond Multi-Purpose-SBMP and Single Bond 2-SB2) and two self-etch adhesives (Clearfil SE Bond-CSE, and Clearfil S3 Bond-CS3) were tested. For SBMP and CSE, the primer was not used. The irradiance and spectral emission of the LCUs were obtained with a radiometer and spectrometer. The materials were placed onto the ATR cell as thin films, the solvent was evaporated (when necessary) and photoactivation was carried out for 20 seconds. The DC (%) was evaluated after five minutes (n = 5). The data were statistically analyzed (p < 0.05). The irradiance for Optilux, Radii, FreeLight 2 and Bluephase was 760, 600, 1000 and 1100 mW.cm(-2), respectively. The wavelength of emission for Optilux was between 375 and 520 nm (peak at 496 nm), while for Radii, it was between 420 and 520 nm (peak at 467 nm). Freelight 2 presented an emission spectrum between 415 and 520 nm, and for Bluephase, it was between 410 and 530 nm, both having a peak at 454 nm. SB2 generally showed higher DC compared with the other bonding agents. When cured using the QTH unit, the DC results were SB2 = CS3 > CSE > SBMP; for all LEDs, the DC results showed SB2 > CSE > SBMP > CS3. For SB2, the highest DC was observed when the material was cured with Radii, while there were no significant differences among the other LCUs. CSE and CS3 showed higher DC when cured using the QTH unit, but similar results were observed among the LEDs. For SBMP, no significant differences among the LCUs were detected. In conclusion, the combination bonding agent vs curing unit had a significant effect on DC, mainly for the self-etch adhesives.
Asunto(s)
Luces de Curación Dental/clasificación , Recubrimientos Dentinarios/efectos de la radiación , Cementos de Resina/efectos de la radiación , Bisfenol A Glicidil Metacrilato/química , Bisfenol A Glicidil Metacrilato/efectos de la radiación , Recubrimientos Dentinarios/química , Humanos , Ensayo de Materiales , Transición de Fase/efectos de la radiación , Procesos Fotoquímicos/efectos de la radiación , Polimerizacion/efectos de la radiación , Radiometría/instrumentación , Cementos de Resina/química , Espectrofotometría/instrumentación , Espectroscopía Infrarroja por Transformada de Fourier , Análisis Espectral , Factores de TiempoRESUMEN
The field dependence of the optical transmission of tartrate-coated and polyaspartate-coated magnetite-based aqueous colloids was studied. The colloidal stock samples were diluted to prepare a series of samples containing different particle volume fractions ranging from 0.17% up to 1.52% and measured at distinct times after preparation (1, 30, 120, 240, and 1460 days). We show that the magneto-transmissivity behavior is mainly described by the rotation of linear chains, at the low-field range, whereas the analysis of the data provided the measurement of the average chain length. Results also reveal that the optical transmissivity has a minimum at a particular critical field, whose origin is related to the onset of columns of chains built from isolated particle chains, i.e., due to a columnar phase transition. We found the critical field reducing as the particle volume fraction increases and as the sample's aging time increases. To investigate the origin of this phenomenon we used phase condensation models and Mie's theory applied to a chain of spheres and to an infinite cylinder. Possible implications for magnetophotonic colloidal-based devices and biomedical applications were discussed.
Asunto(s)
Materiales Biocompatibles/química , Materiales Biocompatibles/efectos de la radiación , Óxido Ferrosoférrico/química , Óxido Ferrosoférrico/efectos de la radiación , Modelos Químicos , Simulación por Computador , Impedancia Eléctrica , Campos Electromagnéticos , Magnetismo , Transición de Fase/efectos de la radiaciónRESUMEN
The use of liposomes to encapsulate materials has received widespread attention for drug delivery, transfection, diagnostic reagent, and as immunoadjuvants. Phospholipid polymers form a new class of biomaterials with many potential applications in medicine and research. Of interest are polymeric phospholipids containing a diacetylene moiety along their acyl chain since these kinds of lipids can be polymerized by Ultra-Violet (UV) irradiation to form chains of covalently linked lipids in the bilayer. In particular the diacetylenic phosphatidylcholine 1,2-bis(10,12-tricosadiynoyl)-sn-glycero-3-phosphocholine (DC8,9PC) can form intermolecular cross-linking through the diacetylenic group to produce a conjugated polymer within the hydrocarbon region of the bilayer. As knowledge of liposome structures is certainly fundamental for system design improvement for new and better applications, this work focuses on the structural properties of polymerized DC8,9PC:1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) liposomes. Liposomes containing mixtures of DC8,9PC and DMPC, at different molar ratios, and exposed to different polymerization cycles, were studied through the analysis of the electron spin resonance (ESR) spectra of a spin label incorporated into the bilayer, and the calorimetric data obtained from differential scanning calorimetry (DSC) studies. Upon irradiation, if all lipids had been polymerized, no gel-fluid transition would be expected. However, even samples that went through 20 cycles of UV irradiation presented a DSC band, showing that around 80% of the DC8,9PC molecules were not polymerized. Both DSC and ESR indicated that the two different lipids scarcely mix at low temperatures, however few molecules of DMPC are present in DC8,9PC rich domains and vice versa. UV irradiation was found to affect the gel-fluid transition of both DMPC and DC8,9PC rich regions, indicating the presence of polymeric units of DC8,9PC in both areas. A model explaining lipids rearrangement is proposed for this partially polymerized system.
Asunto(s)
Materiales Biocompatibles/química , Liposomas/química , Fosfolípidos/química , Procesos Fotoquímicos , Diacetil , Portadores de Fármacos , Transición de Fase/efectos de la radiación , Polímeros , Rayos UltravioletaRESUMEN
Ionising radiation used for sterilization can have an effect on the physicochemical properties of pharmaceutically relevant excipient systems, affecting therefore the stability of the formulation. The effect of gamma irradiation on the phase behaviour (cloud point--CP) and critical micelle concentration (CMC) of aqueous solutions of Triton X-100, used as a model nonionic surfactant, is investigated in this paper. Micellar solutions were irradiated with gamma-rays in a dose range between 0 and 70 kGy, including the sterilization range of pharmaceutical preparations. The decreased observed in CP and CMC values of micellar solutions at all absorbed doses was explained in terms of changes in molecular mass distribution of ethoxylated surfactant and the formation of cross-linked species. These results were complemented by mass spectrometry, UV-vis and NMR spectroscopy. Although the findings indicate degradation of polyethoxylated chains by water radical attacks, there was no spectroscopic evidence of radiation damage to aromatic ring or hydrocarbon tail of surfactant. Models based on Flory-Huggins theory were employed to estimate CP from changes in mass distribution and to obtain cross-linking fractions. Surface tension measurements of non-irradiated and irradiated solutions were used for estimating the effectiveness and efficiency of surfactant in the formulation.