Establishment of a quantitative method for GC analysis of polyoxyethylene (35) castor oil in microemulsion extracts / 中国中药杂志

With the continuous exploration of microemulsions as solvents for traditional Chinese medicine extraction, polyoxyethy-lene(35) castor oil(CrEL), a commonly used surfactant, is being utilized by researchers. However, the problem of detecting residues of this surfactant in microemulsion extracts has greatly hampered the further development of microemulsion solvents. Based on the chemical structures of the components in CrEL and the content determination method of castor oil in the 2020 edition of the Chinese Pharmacopoeia(Vol. Ⅳ), this study employed gas chromatography(GC) and single-factor experiments to optimize the preparation method of methyl ricinoleate from CrEL. The conversion coefficient between the two was validated, and the optimal sample preparation method was used to process microemulsion extracts of Zexie Decoction from three batches. The content of methyl ricinoleate generated was determined, and the content of CrEL in the microemulsion extracts of Zexie Decoction was calculated using the above conversion coefficient. The results showed that the optimal preparation method for CrEL was determined. Specifically, 10 mL of 1 mol·L~(-1) KOH-methanol solution was heated at 60 ℃ for 15 min in a water bath. Subsequently, 10 mL of boron trifluoride etherate-methanol(1∶3) solution was heated at 60 ℃ for 15 min in a water bath, followed by extraction with n-hexane twice. CrEL could stably produce 20.84% methyl ricinoleate. According to this conversion coefficient, the average mass concentration of CrEL in the three batches of Zexie Decoction microemulsion extracts was 11.94 mg·mL~(-1), which was not significantly different from the CrEL mass concentration of 11.57 mg·mL~(-1) during microemulsion formulation, indicating that the established content determination method of this study was highly accurate, sensitive, and repeatable. It can be used for subsequent research on microemulsion extracts of Zexie Decoction and provide a reference for quality control of other drug formulations containing CrEL.

Modification of polyetheretherketone (PEEK) physical features to improve osteointegration / 浙江大学学报（英文版）（B辑：生物医学和生物技术）

Polyetheretherketone (PEEK) has been widely applied in orthopedics because of its excellent mechanical properties, radiolucency, and biocompatibility. However, the bioinertness and poor osteointegration of PEEK have greatly limited its further application. Growing evidence proves that physical factors of implants, including their architecture, surface morphology, stiffness, and mechanical stimulation, matter as much as the composition of their surface chemistry. This review focuses on the multiple strategies for the physical modification of PEEK implants through adjusting their architecture, surface morphology, and stiffness. Many research findings show that transforming the architecture and incorporating reinforcing fillers into PEEK can affect both its mechanical strength and cellular responses. Modified PEEK surfaces at the macro scale and micro/nano scale have positive effects on cell-substrate interactions. More investigations are necessary to reach consensus on the optimal design of PEEK implants and to explore the efficiency of various functional implant surfaces. Soft-tissue integration has been ignored, though evidence shows that physical modifications also improve the adhesion of soft tissue. In the future, ideal PEEK implants should have a desirable topological structure with better surface hydrophilicity and optimum surface chemistry.

Reactive aqueous two-phase systems for the production and purification of PEGylated proteins

BACKGROUND PEGylation, defined as the covalent attachment of polyethylene glycol, allows the synthesis of PEGylated therapeutic proteins with enhanced physicochemical properties. Traditional alkylating Nterminal PEGylation reactions on amine groups involve the use of modified linear mono-methoxy polyethylene glycol (mPEG) molecules looking for the synthesis of mono-PEGylated products. However, this approach requires different purification steps since inevitably undesired cross-linked products are synthesized. Herein, we propose the use of reactive aqueous two-phase systems (ATPS) to produce and purify PEGylated therapeutic conjugates using Ribonuclease A (RNase A) as a model protein. RESULTS: Selected linear 5 kDa and 20 kDa mPEG ­ potassium phosphate systems were produced according to equilibrium data obtained from constructed binodal curves. All reactive systems were able to generate biphasic systems and to PEGylate RNase A. Two 5 kDa and two 20 kDa systems were selected based on the reaction yield percentage and the feasibility of purifying the mono-PEGylated RNase A from the diPEGylated and native RNase A by contrasting the differences in their partition behaviors. The remnant biological activity was of 94% and of 100% for the mono-PEGylated RNase A purified from the 5 kDa and 20 kDa mPEG systems when compared to the mono-PEGylated conjugate obtained by standard procurement methods.

Resin-dentin bond stability of etch-and-rinse adhesive systems with different concentrations of MMP inhibitor GM1489

Abstract Enzymatic degradation of the hybrid layer can be accelerated by the activation of dentin metalloproteinases (MMP) during the bonding procedure. MMP inhibitors may be used to contain this process. Objective To evaluate the degree of conversion (DC%), dentin bond strength (µTBS) (immediate and after 1 year of storage in water), and nanoleakage of an experimental (EXP) and a commercial (SB) adhesive system, containing different concentrations of the MMP inhibitor GM1489: 0, 1 µM, 5 µM and 10 µM. Methodology DC% was evaluated by FT-IR spectroscopy. Dentin bond strength was evaluated by µTBS test. Half of beams were submitted to the µTBS test after 24 h and the other half, after storage for 1 year. From each tooth and storage time, 2 beams were reserved for nanoleakage testing. Data were analyzed using ANOVA and Tukey's test to compare means (α=0.05). Results All adhesive systems maintained the µTBS after 1 year of storage. Groups with higher concentrations of inhibitor (5 µM and 10 µM) showed higher µTBS values than groups without inhibitor or with 1 µM. The nanoleakage values of all groups showed no increase after 1 year of storage and values were similar for SB and EXP groups, in both storage periods. The inhibitor did not affect the DC% of the EXP groups, but the SB5 and SB10 groups showed higher DC% values than those of SB0 and SB1. Conclusions The incorporation of GM1489 in the adhesive systems had no detrimental effect on DC%. The concentrations of 5 µM GM1489 for SB and 5 µM or 10 µM for EXP provided higher μTBS than groups without GM1489, in the evaluation after 1 year of storage; whereas the concentration of inhibitor did not affect adhesive systems nanoleakage.

PLA/PGA and its co-Polymers in Alveolar Bone Regeneration. A Systematic Review / PLA/PGA y sus Copolímeros en Regeneración Ósea Alveolar. Una Revisión Sistemática

ABSTRACT: The aim of this research was to perform a systematic review to identify the most frequent uses of PLA/ PGA in alveolar bone regeneration and their results. A study was designed to answer the question: What are the most frequent uses of PLA/PLGA and their copolymers in alveolar bone regeneration?. A systematic search was done on MEDLINE, EMBASE and LILACS from April 1993 to December 2017. The search string used on MEDLINE was: (((polylactic acid) OR PLA) OR PLA-based copolymers) OR PLA blends) OR PLA scaffolds)) AND ((("Bone Regeneration"[Mesh]) OR bone regeneration) OR guided bone regeneration). The search was complemented by a manual review of the references from the articles included. Most of the studies selected were weak and, regarding the most frequent uses of PLA/PGA, 13 studies used it as a resorbable membrane, two as an absorbable mesh, one as an absorbable screw and three as filling material. Based on our results, the authors consider that PLA/PGA requires a delicate relation between the mechanical resistance and the degradation process. PLA/PGA does not interrupt bone regeneration; however, the influence in cellular events related to bone regeneration and later osseointegration have not been identified.

RESUMEN: El objetivo de esta revisión fue realizar una revisión sistemática de la literatura para identificar los usos más frecuentes de PLA/PGA en regeneración ósea en área maxilofacial y sus resultados. Se diseñó un estudio para responder a la pregunta: ¿Cuáles son los usos más frecuentes de PLA/PLGA y sus copolímeros en regeneración ósea en el sector maxilofacial?. Los estudios seleccionados fueron en su mayoría débiles y sobre los usos más frecuentes de PLA/PGA, 13 estudios lo utilizaron como membrana reabsorbible, 2 estudios como malla absorbible, un estudio como tornillo absorbible y 3 estudios como material de relleno. En base a nuestros resultados, los autores estiman que PLA/PGA requiere una delicada relación entre la resistencia mecánica que ofrece y la degradación que se produce; PLA/ PGA no interrumpe la regeneración ósea, sin embargo, no se ha identificado la potencialidad o influencia que presenta en los eventos celulares de la regeneración y posterior oseointegración.

Synthesis, characterization, and in vitro evaluation of gamma radiationinduced PEGylated isoniazid

Background: The search for innovative anti-tubercular agents has received increasing attention in tuberculosis chemotherapy because Mycobacterium tuberculosis infection has steadily increased over the years. This underlines the necessity for new methods of preparation for polymer-drug adducts to treat this important infectious disease. The use of poly(ethylene glycol)(PEG) is an alternative producing anti-tubercular derivatives. However, it is not yet known whether PEGylated isonicotinylhydrazide conjugates obtained by direct links with PEG are useful for therapeutic applications. Results: Here, we synthesized a PEGylated isoniazid (PEG-g-INH or PEG­INH) by gamma radiation-induced polymerization, for the first time. The new prodrugs were characterized using Raman and UV/Vis spectrometry. The mechanism of PEGylated INH synthesis was proposed. The in vitro evaluation of a PEGylated isonicotinylhydrazide macromolecular prodrug was also carried out. The results indicated that PEG­INH inhibited the bacterial growth above 95% as compared with INH, which showed a lower value (80%) at a concentration of 0.25 µM. Similar trends are observed for 0.1, 1, and 5 µM. Conclusions: In summary, the research suggests that it is possible to covalently attach the PEG onto INH by the proposed method and to obtain a slow-acting isoniazid derivative with little toxicity in vitro and higher antimycobacterial potency than the neat drug.

Effect of iodonium salt and chitosan on the physical and antibacterial properties of experimental infiltrants

Abstract Resinous infiltrants are indicated in the treatment of incipient carious lesions, and further development of these materials may contribute to greater control of these lesions. The aim of this study was to analyze the physical and antibacterial properties of experimental infiltrants containing iodonium salt and chitosan. Nine experimental infiltrants were formulated by varying the concentration of the diphenyliodonium salt (DPI) at 0, 0.5 and 1 mol%; and chitosan at 0, 0.12 and 0.25 g%. The infiltrants contained the monomeric base of triethylene glycol dimethacrylate and bisphenol-A dimethacrylate ethoxylate in a 75 and 25% proportion by weight, respectively; 0.5 mol% camphorquinone and 1 mol% ethyl 4-dimethylaminobenzoate. The degree of conversion was evaluated using Fourier transformer infrared spectroscopy, and the flexural strength and elastic modulus using the three-point bending test. Sorption and solubility in water, and antibacterial analysis (minimum inhibitory concentration and minimum bactericidal concentration) were also analyzed. Data was analyzed statistically by two-way ANOVA and Tukey's test (p<0.05), with the exception of the antibacterial test, which was evaluated by visual inspection. In general, the infiltrant group containing 0.5% DPI and 0.12% chitosan showed high values of degree of conversion, higher values of elastic modulus and flexural strength, and lower sorption values in relation to the other groups. Antibacterial activity was observed in all the groups with DPI, regardless of the concentration of chitosan. The addition of DPI and chitosan to experimental infiltrants represents a valid option for producing infiltrants with desirable physical and antibacterial characteristics.

Influence of activation mode, fatigue, and ceramic interposition on resin cements' diametral tensile strength

Abstract This study evaluated the influence of activation modes, on Diametral Tensile Strength (DTS) of dual cured resin cements subjected to a Mechanical Fatigue test (MF). Four dual-cured resin cements (RelyX UNICEM [U], RelyX ARC [A], ENFORCE [E] and Nexus 2 [N]) were activated by three different curing modes as follows: Self-Curing (SC), Dual Cure activation with photoactivation executed directly (DC) and Dual Cure activation with Photoactivation Through Porcelain (DCTP). After 24 hours, half of the sample was subjected to 30.000 fatigue cycles at 1 Hz frequency and 12 N load. Then, all specimens were subjected to DTS test in Instron Universal Testing Machine and data were analyzed by three-way ANOVA and Tukey's Test (5%). The results of DTS test means (MPa) and standard deviation, for each cement factor activated by SC, DC and DCTP was respectively: U (28.12 ± 5.29; 37.44 ± 6.49 and 40.10 ± 4.39), A (49.68 ± 8.42; 55.12 ± 5.16 and 63.43 ± 6.92), E (49.12 ± 3.89; 56.42 ± 8.88 and 56.96 ± 6.45) and N (61.89 ± 11.21; 59.26 ± 9.47 and 62.56 ± 10.93). Turkey's test indicated that DC is related to the highest DTS values; Nexus 2 DTS remained the same independently of activation mode and that the Porcelain disk interposition enhanced DTS only for RelyX ARC the ANOVA statistical test indicated that MF didn't alter the DTS values for all experimental groups. MF results clinical implication is that all cements tested exhibited, in an immediate loading, good cross linked bonds quality.

Doxycycline release and antibacterial activity from PMMA/PEO electrospun fiber mats

Abstract Objective: To investigate the use of polymethyl methacrylate (PMMA) electrospun fiber mats containing different amounts of polyethylene oxide (PEO) as a doxycycline delivery system and to test antibacterial activity against an oral pathogen. Methodology: PMMA powders or PEO (mol wt 200 Kd) (10,20,30% w/w/) were dissolved in N, N-dimethylformamide (DMF) to obtain a final polymer concentration of 15% in DMF (w/v). 2% Doxycycline monohydrate was added to the solutions and submitted to vortex mixing. The solution was transferred to a plastic syringe and fit into a nanofiber electrospinning unit. The parameters applied were: voltage at 17.2 kV; distance of 20 cm between the needle tip and the collector plate; target speed at 2 m/min; and transverse speed at 1cm/min. Syringe pump speed was 0.15 mm/min. The drug release analysis was performed by removing aliquots of the drug-containing solution (in PBS) at specific periods. Doxycycline release was quantified using RP-HPLC. Fiber mats from all groups had their antibacterial action tested against S. mutans based on inhibition halos formed around the specimens. The experiments were performed in triplicate. Gravimetric analysis at specific periods was performed to determine any polymer loss. Morphological characterization of the electrospun fibers was completed under an optical microscope followed by SEM analysis. Results: The addition of PEO to the PMMA fibers did not affect the appearance and diameter of fibers. However, increasing the %PEO caused higher doxycycline release in the first 24 h. Fibers containing 30% PEO showed statistically significant higher release when compared with the other groups. Doxycycline released from the fibers containing 20% or 30% of PEO showed effective against S. mutans. Conclusion: The incorporation of PEO at 20% and 30% into PMMA fiber mat resulted in effective drug release systems, with detected antibacterial activity against S. mutans.

Enhanced water solubility, antioxidant activity, and oral absorption of hesperetin by D-α-tocopheryl polyethylene glycol 1000 succinate and phosphatidylcholine / 浙江大学学报（英文版）（B辑：生物医学和生物技术）

Hesperetin, an abundant bioactive component of citrus fruits, is poorly water-soluble, resulting in low oral bioavailability. We developed new formulations to improve the water solubility, antioxidant activity, and oral absorption of hesperetin. Two nano-based formulations were developed, namely hesperetin-TPGS (D-α-tocopheryl polyethylene glycol 1000 succinate) micelles and hesperetin-phosphatidylcholine (PC) complexes. These two formulations were prepared by a simple technique called solvent dispersion, using US Food and Drug Administration (FDA)-approved excipients for drugs. Differential scanning calorimetry (DSC) and dynamic light scattering (DLS) were used to characterize the formulations' physical properties. Cytotoxicity analysis, cellular antioxidant activity assay, and a pharmacokinetic study were performed to evaluate the biological properties of these two formulations. The final weight ratios of both hesperetin to TPGS and hesperetin to PC were 1:12 based on their water solubility, which increased to 21.5- and 20.7-fold, respectively. The hesperetin-TPGS micelles had a small particle size of 26.19 nm, whereas the hesperetin-PC complexes exhibited a larger particle size of 219.15 nm. In addition, the cellular antioxidant activity assay indicated that both hesperetin-TPGS micelles and hesperetin-PC complexes increased the antioxidant activity of hesperetin to 4.2- and 3.9-fold, respectively. Importantly, the in vivo oral absorption study on rats indicated that the micelles and complexes significantly increased the peak plasma concentration (Cmax) from 2.64 μg/mL to 20.67 and 33.09 μg/mL and also increased the area under the concentration-time curve of hesperetin after oral administration to 16.2- and 18.0-fold, respectively. The micelles and complexes increased the solubility and remarkably improved the in vitro antioxidant activity and in vivo oral absorption of hesperetin, indicating these formulations' potential applications in drugs and healthcare products.

Long-term bonding efficacy of adhesives containing benzodioxioles as alternative co-initiators

Abstract This study evaluated the three-year lifespan of the bond to dentin of experimental self-etch adhesives containing benzodioxole derivatives - 1,3-benzodioxole (BDO) and piperonyl alcohol (PA) - as co-initiator alternative to amines. Adhesive resins were formulated using Bis-GMA, TEGDMA, HEMA, camphorquinone and different co-initiators: BDO, PA or ethyl 4-dimethylamino benzoate (EDAB - amine). An experimental self-etch primer was used to complete the two-step, self-etch adhesive system. Clearfil SE Bond (CSE) was used as commercial reference. Bond strength to human dentin was assessed by microtensile bond strength (µTBS) test, and failure mode was classified. Morphology of the dentin bonding interface was assessed via scanning electron microscopy (SEM). Irrespective of the dental adhesives evaluated, µTBS was higher after 24 hours compared with that after 1.5 and 3 years (p ≤ 0.001). However, adhesives with BDO and PA as co-initiators showed significantly higher bond strength than the bonding resin with EDAB (p ≤ 0.002), independent of the time evaluated. The commercial adhesive CSE showed similar bond strength compared with the other groups (p ≥ 0.05). Mixed failures were mainly observed after 24 hours, while adhesive failures were more frequently observed after 1.5 and 3 years. No notable differences in homogeneity and continuity along the bonded interfaces were detected among the materials in the SEM analysis. In conclusion, benzodioxole derivatives are feasible alternative co-initiators to tertiary amine in camphorquinone-based self-etching dental adhesive formulations.

Model resin composites incorporating ZnO-NP: activity against S. mutans and physicochemical properties characterization

Abstract Although resin composites are widely used in the clinical practice, the development of recurrent caries at composite-tooth interface still remains as one of the principal shortcomings to be overcome in this field. Objectives To evaluate the activity against S. mutans biofilm of model resin composites incorporating different concentrations of ZnO-nanoparticles (ZnO-NP) and characterize their physicochemical properties. Materials and Methods Different concentrations of ZnO-NP (wt.%): E1=0, E2=0.5, E3=1, E4=2, E5=5 and E6=10 were incorporated into a model resin composite consisting of Bis-GMA-TEGDMA and barium borosilicate particles. The activity against S. mutans biofilm was evaluated by metabolic activity and lactic acid production. The following physicochemical properties were characterized: degree of conversion (DC%), flexural strength (FS), elastic modulus (EM), hardness (KHN), water sorption (Wsp), water solubility (Wsl) and translucency (TP). Results E3, E4, E5 and E6 decreased the biofilm metabolic activity and E5 and E6 decreased the lactic acid production (p<0.05). E6 presented the lowest DC% (p<0.05). No significant difference in FS and EM was found for all resin composites (p>0.05). E5 and E6 presented the lowest values of KHN (p<0.05). E6 presented a higher Wsp than E1 (p<0.05) and the highest Wsl (p<0.05). The translucency significantly decreased as the ZnO- NP concentration increased (p<0.05). Conclusions The incorporation of 2 - 5 wt.% of ZnO-NP could endow antibacterial activity to resin composites, without jeopardizing their physicochemical properties.

Degree of conversion and bond strength of resin-cements to feldspathic ceramic using different curing modes

Abstract Resin cements have led to great advances in dental ceramic restoration techniques because of their ability to bond to both dental structures and restorative materials. Objective The aim of this study was to assess the performance of resin cements when different curing modes are used, by evaluating the degree of conversion and bond strength to a ceramic substrate. Material and Methods Three resin cements were evaluated, two dual-cured (Variolink II and RelyX ARC) and one light-cured (Variolink Veneer). The dual-cured resin cements were tested by using the dual activation mode (base and catalyst) and light-activation mode (base paste only). For degree of conversion (DC) (n=5), a 1.0 mm thick feldspathic ceramic disc was placed over the resin cement specimens and the set was light activated with a QTH unit. After 24 h storage, the DC was measured with Fourier transform infrared spectroscopy (FTIR). For microshear bond strength testing, five feldspathic ceramic discs were submitted to surface treatment, and three cylindrical resin cement specimens were bonded to each ceramic surface according to the experimental groups. After 24 h, microshear bond testing was performed at 0.5 mm/min crosshead speed until the failure. Data were submitted to one-way ANOVA followed by Tukey test (p<0.05). Scanning electron microscopy (SEM) was used for classifying the failure modes. Results Higher DC and bond strength values were shown by the resin cements cured by using the dual activation mode. The Variolink II group presented higher DC and bond strength values when using light-activation only when compared with the Variolink Veneer group. Conclusion The base paste of dual-cured resin cements in light-activation mode can be used for bonding translucent ceramic restorations of up to or less than 1.0 mm thick.

Influence of addition of [2-(methacryloyloxy)ethyl]trimethylammonium chloride to an experimental adhesive

Abstract The aim of this study was to develop an experimental adhesive with addition of [2-(methacryloyloxy)ethyl]trimethylammonium chloride (METAC) and to evaluate its mechanical and biological properties and its in vitro antibacterial activity. An experimental adhesive resin was formulated with Bis-GMA, TEGDMA, and HEMA. The antibacterial monomer was added at concentrations of 1%, 2.5%, and 5% (METAC groups). A group without METAC addition was used as control. The experimental adhesives were evaluated as to their antibacterial potential against Streptococcus mutans, degree of conversion, and softening in ethanol for 2 hours. The data were analyzed by one-way ANOVA, Tukey’s post-hoc test, and the paired Student’s t-test (significance level of 0.05). METAC showed antibacterial activity against S. mutans at all concentrations (p < 0.05). There was no statistical difference across METAC groups (p > 0.05). The 1%, 2.5%, and 5% groups yielded the highest mean values for degree of conversion (p < 0.05). The 1% group did not differ from the control group (p > 0.05). There was no statistical difference in baseline microhardness values (p > 0.05) and microhardness values after immersion in ethanol were lower than at baseline for all groups (p < 0.05). There was no statistical difference in the reduction of Knoop hardness number (KHN) after immersion in ethanol for any of the groups (p > 0.05). The results of the present study indicate that METAC is a promising antibacterial agent when added to an adhesive system.

Longevity of metal-ceramic crowns cemented with self-adhesive resin cement: a prospective clinical study

Abstract Resin cements are often used for single crown cementation due to their physical properties. Self-adhesive resin cements gained widespread due to their simplified technique compared to regular resin cement. However, there is lacking clinical evidence about the long-term behavior of this material. The aim of this prospective clinical trial was to assess the survival rates of metal-ceramic crowns cemented with self-adhesive resin cement up to six years. One hundred and twenty-nine subjects received 152 metal-ceramic crowns. The cementation procedures were standardized and performed by previously trained operators. The crowns were assessed as to primary outcome (debonding) and FDI criteria. Statistical analysis was performed using Kaplan-Meier statistics and descriptive analysis. Three failures occurred (debonding), resulting in a 97.6% survival rate. FDI criteria assessment resulted in scores 1 and 2 (acceptable clinical evaluation) for all surviving crowns. The use of self-adhesive resin cement is a feasible alternative for metal-ceramic crowns cementation, achieving high and adequate survival rates.

Evaluation of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental dental resin-based materials

ABSTRACT Objective To evaluate the influence of phenyl-propanedione on yellowing and chemical-mechanical properties of experimental resin-based materials photoactivated using different light curing units (LCUs). Material and Methods Experimental resin-based materials with the same organic matrix (60:40 wt% BisGMA:TEGDMA) were mechanically blended using a centrifugal mixing device. To this blend, different photoinitiator systems were added in equimolar concentrations with aliphatic amine doubled by wt%: 0.4 wt% CQ; 0.38 wt% PPD; or 0.2 wt% CQ and 0.19 wt% PPD. The degree of conversion (DC), flexural strength (FS), Young’s modulus (YM), Knoop hardness (KNH), crosslinking density (CLD), and yellowing (Y) were evaluated (n=10). All samples were light cured with the following LCUs: a halogen lamp (XL 2500), a monowave LED (Radii), or a polywave LED (Valo) with 16 J/cm2. The results were analysed by two-way ANOVA and Tukey’s test (α=0.05). Results No statistical differences were found between the different photoinitiator systems to KNH, CLS, FS, and YM properties (p≥0.05). PPD/CQ association showed the higher DC values compared with CQ and PPD isolated systems when photoactivated by a polywave LED (p≤0.05). Y values were highest for the CQ compared with the PPD systems (p≤0.05). Conclusion PPD isolated system promoted similar chemical and mechanical properties and less yellowing compared with the CQ isolated system, regardless of the LCU used.

Effects of the application techniques of self-adhesive resin cements on the interfacial integrity and bond strength of fiber posts to dentin

ABSTRACT Objective: To evaluate the influence of an application technique of a glass-fiber post using self-adhesive resin cements on the push-out bond strength and the presence of bubbles in the root thirds. The cements were either applied according to the manufacturer's instruction or using a commercial delivering system (Centrix), at which the cement pastes were collected and applied after manipulation. Material and Methods: Self-adhesive resin cements (RelyX U200/3M ESPE-U200; Maxcem Elite/Kerr-MAX; Clearfil SA Cement/Kuraray-CSA) and a conventional cement (RelyX ARC/3M ESPE-ARC) were used to cement a post and applied either based on the manufacturer's instructions or using a Centrix syringe to deliver the cements directly onto the post of choice, or directly into canal. The roots were scanned with a micro-computed tomography (μCT) and then sectioned into nine 1-mm thick slices for a push-out bond strength test. The μCT images showed the percentage of bubbles in the root thirds (cervical, medium, and apical). Data were analyzed with three-way ANOVA/Tukey (α=0.05). Results: Triple interaction was not significant (p>0.05). The interaction “material” vs “root third” was not significant. A significant interaction was observed between “material” vs “application technique” (p<0.05). For ARC, U200, and MAX, significantly lower percentages of bubbles were observed when the Centrix syringe delivered the cements. Equivalent percentages of voids were observed for CSA, irrespective of the application technique (p>0.05). Significantly higher bond strength was observed when the self-adhesive resin cements were applied using the Centrix delivery system, in comparison with the manufacturer's instructions (p<0.05). Bond strength varied with the root third: cervical>medium>apical (p<0.05). No correlations were found between the bond strength and voids. Conclusions: Bond strength and voids are negatively influenced by the conventional application technique for luting fiber posts. The delivery system (Centrix) seems to produce better results when cementing fiber posts.

Influência na resistência de união de pinos de fibra de vidro com e sem retenções mecânicas em função dos materiais utilizados para cimentação: teste de 'push-out' / Influence on the bond strength of glass fiber posts with and without mechanical retentions depending of materials used for cementing: push-out test

Este estudo teve como objetivo avaliar a influência na resistência de união de pinos de fibra de vidro (PFV) com retenções mecânicas (CRM) e sem retenções (SR), associados a três materiais: RelyX ARC cimento resinoso convencional dual com sistema adesivo Adper Single Bond (ASB), convencional de 2 passos; RelyX U200 cimento resinoso auto condicionante dual e resina flow SDR foto ativada, com sistema adesivo Prime & Bond 2.1 (PB), convencional de 2 passos; nos terços cervical (C), médio (M) e apical (A), por meio do teste de push-out. Sessenta incisivos bovinos foram selecionados, tiveram as coroas seccionadas para padronizar 17mm de raiz e foram submetidas ao tratamento endodôntico, para posterior cimentação do PFV. Foram divididas aleatoriamente em 2 grupos (N=30), quanto ao tipo de PFV: CRM - com retenções mecânicas (Glassix+plus no2) e SR - sem retenções (Exacto no2). Todos os PFV apresentavam formato cônico. Cada grupo foi subdividido em 3 (N=10), quanto ao tipo de material: cimento RelyX ARC+ASB; cimento RelyX U200 (auto condicionante) e resina SDR+PB. Todas as orientações dos fabricantes para tempo de manipulação e foto ativação do material foram rigorosamente respeitadas. As raízes foram mantidas em saliva artificial e decorridas 24h da cimentação dos PFV, foram seccionadas perpendicularmente ao longo eixo, obtendo 9 fatias de aproximadamente 1mm, cuja identificação foi feita de acordo com o terço correspondente. O teste de push-out foi realizado em máquina de ensaio universal com célula de carga de 50N; velocidade de 0,5mm/min, da direção apical para a cervical da fatia até que o pino fosse deslocado, respeitando o formato cônico do canal radicular. Todos os espécimes foram analisados em microscopia óptica, aumento de 200 vezes, quanto aos tipos de falha ocorrido. Os dados foram tabulados considerando as variáveis dos diferentes materiais utilizados para a cimentação, presença ou não de retenções mecânicas nos PFV e terços radiculares. Os valores de resistência de união (Ru) obtidos foram submetidos ao teste de normalidade Kolmogorov- Smirnov, à análise de variância a três critérios (ANOVA) e ao teste LSD de Fisher (p<0,05). Os resultados mostraram diferença estatisticamente significante nos terços C, M e A, respectivamente para os cimentos ARC com pino Glassix+plus, média e desvio padrão (MPa) a seguir, 8,50 (4,76); 6,99 (3,55); 4,71 (2,13) e U200 com pino Exacto: 9,40 (4,93); 8,02 (4,67); 4,67 (1,86); a resina SDR não interagiu significativamente com os PFV CRM 6,78 (2,72); 5,97 (2,45); 2,67 (1,55) e SR 7,24 (3,55); 6,86 (2,84); 4,10 (1,90). A análise microscópica mostrou predominância de falhas adesivas entre cimento e dentina e mista para todos os grupos. O cimento U200 com pino Exacto apresentou o melhor desempenho, seguido do ARC com pino Glassix+plus. A resina SDR teve desempenho semelhante para ambos os PFV. Todos os grupos apresentaram valores de Ru maiores no terço cervical, intermediários no terço médio e menores no terço apical.(AU)

This study aimed to evaluate the influence on the bond strength of glass fiber posts (GFP) with mechanical retention (WMR) and without retentions (NR), associated with three materials: RelyX ARC total-etching resin cement dual cure with Adper Single Bond (ASB) adhesive system, conventional 2 steps; RelyX U200 self-etching resin cement dual cure, and flowable resin SDR, activated by light, with Prime & Bond 2.1 adhesive system conventional 2 steps in the cervical (C), medium (M) and apical (A) thirds by the "push-out" test. Were selected sixty bovine incisors, had the crowns sectioned to root was standardized 17mm, were submitted to endodontic treatment, for cementing the GFP later. Were randomly divided into 2 groups (N=30), according to the GFP: WMR - with mechanical retentions (Glassix+plus ≠2) and NR - without retentions (Exacto ≠2). All GFP had conic shape. Each group was divided into 3 (N=10), according to material: RelyX ARC+ASB, RelyX U200 (self-etching) and flowable resin SDR+PB. All guidelines of manufacturers to handling time and cure time of the material were strictly adhered. The roots were kept in artificial saliva and 24 hours after GFP cementing it were sectioned perpendicular to the long axis, obtaining nine slices of approximately 1mm, which identification was done according to the corresponding third. The "push-out" test was performed with a universal test machine, 50N load cell; crosshead speed of 0.5 mm/min, the load was applied in an apical to cervical direction until the post dislodged from the specimen, respecting the conical shape of the root canal. Subsequently, all specimens were analyzed with optical microscopy 200 times increase to evaluate failure modes. Data were tabulated considering the materials used for cementing, presence or absence of mechanical retentions in GFP and root thirds. The bond strength values (BS) were submitted to Kolmogorov-Smirnov normality test, three-way ANOVA and Fisher's LSD test (p<0.05). The values showed statistically significant differences in thirds C, M and A, respectively for the ARC with Glassix+plus, average and standard deviation (MPa): 8.50 (4.76); 6.99 (3.55); 4.71 (2.13) and U200 with Exact post: 9.40 (4.93); 8.02 (4.67); 4.67 (1.86). SDR resin does not significantly interacted with GFP WMR 6.78 (2.72); 5.97 (2.45); 2.67 (1.55) and NR 7.24 (3.55); 6.86 (2.84); 4.10 (1.90). The microscopic analysis showed predominance of failure between cement and dentine and mixed for all groups. U200 cement with Exacto post had the best performance, followed by ARC with Glassix+plus post, SDR resin has similar performance for both GFP. All groups showed BS values higher in the cervical third, intermediate in the middle third and smaller in the apical third.(AU)

Optimizing light-cured composite through variations in camphorquinone and butylhydroxytoluene concentrations

Abstract The use of a free-radical polymerization inhibitor, butylhydroxytoluene (BHT), and a common photo-initiator, camphorquinone (CQ), to reduce polymerization stress in dental composite was investigated in this study. Samples were prepared by mixing Bis-GMA, UDMA, and TEGDMA at a 1:1:1 ratio (wt%), and silanized borosilicate glass fillers at 70 wt% were added to form the composite. Sixteen groups of resin composite were prepared using combinations of four CQ (0.1%, 0.5%, 1.0%, and 1.5%) and four BHT (0.0%, 0.5%, 1.0%, and 1.5%) concentrations. For each group, six properties were tested, including flexural strength (FS), flexural modulus (FM), degree of conversion (DC), contraction stress (CS), stress rate, and gel point (GP). The effects of CQ and BHT combinations on each of these properties were evaluated using two-way analysis of variance (ANOVA) and Fisher's Protected Least Significant Differences test at the 5% significance level. Groups with low CQ and BHT showed moderate values for FS, FM, and CS with a 70% DC. Increasing the BHT concentration caused a decrease in CS and DC with an increase in GP values. Increasing the CQ content led to a steady increase in values for FS and FM. High CQ and BHT combinations showed the most promising values for mechanical properties with low stress values.

Relined fiberglass post: an ex vivo study of the resin cement thickness and dentin-resin interface

Abstract The aim of this study was to evaluate the thickness of resin cements in the root thirds when using conventional fiberglass posts (CP) and relined fiberglass posts (RP) in weakened roots and to evaluate the morphological characteristics of the dentin-resin interface. Forty human maxillary anterior teeth had the crown sectioned below the cemento-enamel junction. The canals were endodontically treated and weakened with diamond burs. Teeth were divided into four groups (n = 10): Group 1 - CP + RelyX ARC; Group 2 - CP + RelyX U200; Group 3 - RP + RelyX ARC; and Group 4 - RP + RelyX U200. Prior to luting, 0.1% Fluorescein and 0.1% Rhodamine B dyes were added to an adhesive and resin cement, respectively. Slices were obtained from the apical, middle, and cervical thirds of the root. Confocal laser scanning microscopy images were recorded in four areas (buccal, lingual, mesial, distal) of each third. In each area, four equidistant measures of the resin cement were made and the mean value was calculated. The interface morphology was observed. The data were submitted to three-way ANOVA and Tukey's test (α = 0.05). The interaction between fiberglass posts, resin cement, and root thirds was significant (p < 0.0001). The resin cement thicknesses were significantly lower for RP in comparison with CP, except in the apical third. There was no significant difference between the resin cements for RP. There was formation of resin cement tags and adhesive tags along the root for RP. RP favored the formation of thin and uniform resin cement films and resin tags in weakened roots.