Is additional silane application necessary for a new silane-containing universal adhesive to bond to glass ceramics?

OBJECTIVE: To evaluate the in vitro influence of prior silane application on the microshear bond strength (µSBS) of Scotchbond Universal Plus to glass ceramic. MATERIALS AND METHODS: Thirty blocks of lithium disilicate ceramic were etched with hydrofluoric acid for 20 s and distributed into Group 1 (no silane and no adhesive), Group 2 (adhesive), Group 3 (silane + adhesive). Three cylinders of resin cement were made on each ceramic block. Five blocks (n = 15 cylinders) were subjected to the µSBS test after 24 h, and the other five blocks (n = 15 cylinders) were tested after 6 months of water storage. RESULTS: According to two-way ANOVA, followed by Tukey's test, the means of µSBS (MPa), denoted by different letters, show significant differences (p < 0.05): after 24 h-Group 1 (31.7)B, Group 2 (43.3)A, and Group 3 (31.3)B; after 6 months-Group 1 (14.8)B, Group 2 (33.6)A, and Group 3 (30.3)A. After 6 months of storage, there was a significant decrease in µSBS for Groups 1 and 2, along with an increase in adhesive failures across all groups. CONCLUSIONS: Prior application of silane did not increase the µSBS between Scotchbond Universal Plus and ceramic, and there was degradation at the bond interface over time. CLINICAL SIGNIFICANCE: Prior application of a silane agent is not necessary when using Scotchbond Universal Plus for bonding to glass ceramics. Regardless of the prior application of silane, there is degradation at the bond interface over time.

Development of silanized bacterial cellulose aerogels for the incorporation of natural oils with healing properties: Copaiba (Copaifera officinalis), bourbon geranium (Pelargonium X ssp.) essential oils and buriti (Mauritia flexuosa) vegetable oil.

Bacterial cellulose (BC) represents a promising biomaterial, due to its unique and versatile properties. We report, herein, on purposely-designed structural modifications of BC that enhance its application as a wound dressing material. Chemical modification of the functional groups of BC was performed initially to introduce a hydrophobic/oleophilic character to its surface. Specifically, silanization was carried out in an aqueous medium using methyltrimethoxisilane (MTMS) as the silanizing agent, and aerogels were subsequently prepared by freeze-drying. The BC-MTMS aerogel obtained displayed a highly porous (99 %) and lightweight structure with an oil absorption capacity of up to 52 times its dry weight. The XRD pattern indicated that the characteristic crystallographic planes of the native BC were maintained after the silanization process. Thermal analysis showed that the thermal stability of the BC-MTMS aerogel increased, as compared to the pure BC aerogel (pBC). Moreover, the BC-MTMS aerogel was not cytotoxic to fibroblasts and keratinocytes. In the second step of the study, the incorporation of natural oils into the aerogel's matrix was found to endow antimicrobial and/or healing properties to BC-MTMS. Bourbon geranium (Pelargonium X ssp.) essential oil (GEO) was the only oil that exhibited antimicrobial activity against the tested microorganisms, whereas buriti (Mauritia flexuosa) vegetable oil (BVO) was non-cytotoxic to the cells. This study demonstrates that the characteristics of the BC structure can be modified, while preserving its intrinsic features, offering new possibilities for the development of BC-derived materials for specific applications in the biomedical field.

Influence of Varied Silane Commercial Brands and Adhesive Application on Bond Strength and Stability to Lithium Disilicate Glass Ceramic.

OBJECTIVES: This study aimed to evaluate the impact of various commercial silane brands with varied chemical compositions with or without the application of an adhesive layer on the microshear bond strength and durability of a resin luting agent to lithium disilicate glass ceramic. METHODS AND MATERIALS: Lithium disilicate glass ceramic discs (EMX, IPS e.max Press, Ivoclar Vivadent) measuring 10 mm in diameter and 3 mm in thickness were fabricated (n=240). Surfaces were etched using 5% hydrofluoric acid and randomly assigned to 10 groups based on the commercial brand of silane used (n=24): [RP] RelyX Ceramic Primer (3M ESPE); [PS] Prosil (FGM); [SA] Silano (Angelus); [SM] Silano (Maquira); [SU] Silane (Ultradent); [GL] GLUMA Ceramic Primer (Kulzer); [CB] Ceramic Bond (VOCO); [MB] Monobond N (Ivoclar Vivadent); [CP] Clearfil Ceramic Primer (Kuraray); and [DE] 2-step silane (Dentsply Sirona). Half of the EMXs (n=12) received a thin adhesive layer (+) after the silane and prior to resin luting agent, while the other half (n=12) did not receive an adhesive layer (-). For the microshear bond strength test (µSBS), four light-cured resin luting agent cylinders (1 mm in diameter) were created on each EMX surface. Half of these specimens were tested after 24 hours, while the other half were stored in deionized water for 6 months. The µSBS test was conducted using a universal testing machine (DL 500, EMIC) at a crosshead speed of 1 mm/min until failure. The obtained data underwent statistical analysis using analysis of variance (ANOVA) and the Tukey test (α=0.05). RESULTS: There was significant influence of the silane commercial brand on bond strength. Notably, "universal primers" yielded lower bond strength results compared to "pure" silane solutions. Water storage had a detrimental effect on microshear bond strength for certain silane commercial brands. Additionally, the application of an adhesive layer negatively impacted bond strength results for all silanes. CONCLUSIONS: This study confirms the importance of both silane commercial brand and chemical composition in relation to bond strength of resin luting agents to lithium disilicate glass ceramic. Furthermore, the application of an adhesive layer may have an adverse effect on bond stability over time.

Surface treatments of the zirconia-reinforced lithium disilicate ceramic in the adhesion to the resin cement.

This study verified the effect of surface treatments of the zirconia-reinforced lithium disilicate ceramic bonded to resin cement. Ceramic blocks were divided according to treatments (n=10): FA+SRX (Fluoric acid + silane RX), FA+MDP (Fluoric acid + MDP), FA+SCF+MDP (Fluoric acid + silane CF + MDP), FA+MEP (Fluoric acid + MEP), and MEP (Self-etch primer). Resin cement cylinders were made in the ceramic blocks, photoactivated with 1,200 mW/cm² for 40s, stored in water at 37°C for 24h, and evaluated by the microshear strength test, optical failure descriptive analysis (%), surface characterization (SEM) and contact angle (Goniometer). Other samples were submitted to 10,000 thermocycles between 5°C and 55°C. Bond strength data were submitted to two-way ANOVA and Tukey's test. Contact angle to one-way ANOVA and Games-Howell's test (5%). At 24h, MEP showed higher bond strength, and FA+SRX the lower. FA+MDP and FA+SCF+MDP showed similar values and FA+MEP was intermediate. After thermocycling, FA+SCF+MDP, FA+MEP, and MEP showed higher values, and FA+SRX the lower while FA+MDP was intermediate. When the periods were compared, FA+MDP, FA+SCF+MDP, FA+MEP, and MEP showed higher values for 24h while FA+SRX was similar. SEM showed retentive surface and crystal exposure when treated with FA+SCF+MDP. The less retentive surface was obtained with MEP, and the other treatments promoted intermediate irregularities. In conclusion, surface treatment and thermocycling promoted different values of adhesive strength and contact angle in a zirconia-reinforced lithium silicate ceramic. Failures were predominantly adhesive, and the ceramic surface was characterized by different levels of roughness and selective exposure of crystals.

Preheated acid associated with silane and electric current in the adhesion of the resin cement to ceramic.

This study verified the effect of the combination of preheated hydrofluoric acid/silane/electric current in the adhesion of the resin cement to ceramic. IPS E.max Press ceramic discs embedded in PVC rigid tubes were divided into four groups associating preheated hydrofluoric acid and silane applied with electrical current (n=10): Ha+S (Heated acid + silane); Ha+S+Ec (Heated acid + silane + electrical current); A+S (Acid + silane) and A+S+Ec (Acid + silano + electrical current). Resin cement/ceramic samples were stored in water at 37°C for 24h. After storage, they were submitted to the microshear test, fracture analysis, and contact angle at 24h or after thermocycling (10,000 cycles/5-55ºC). Bond strength data were evaluated by two-way ANOVA. For comparison between evaluation times (24h or thermocycling) was applied unpaired t-test. A significance post-hoc test of p=0.05 was assumed for analyses and graphs (GraphPad Prism 9.0 software). At 24h, the microshear strength showed similar values between Ha+S, Ha+S+Ec, and A+S+Ec groups, while A+S showed the lowest value with a statistical difference. After thermocycling, Ha+S and Ha+S+Ec were similar, as well as A+S and A+S+Ec. There was a significant difference in all groups comparing 24h (highest value) with after thermocycling (lowest value). Adhesive fracture was predominant in all groups and evaluation times. Ha+S and A+S groups showed higher contact angle values compared to the Ha+S+Ec and A+S+Ec with lower values. In conclusion, the association of preheated hydrofluoric acid/silane applied or not with electric current promoted different microshear strength values, fracture types, and contact angles in the resin cement/ceramic bond.

Revisiting carboxylic group functionalization of silica sol-gel materials.

The carboxylic chemical group is a ubiquitous moiety present in amino acids, a ligand for transition metals, a colloidal stabilizer, and a weak acidic ion-exchanger in polymeric resins and given this property, it is attractive for responsive materials or nanopore-based gating applications. As the number of uses increases, subtle requirements are imposed on this molecular group when anchored to various platforms for the functioning of an integrated chemical system. In this context, silica stands as an inert and multipurpose platform that enables the anchoring of multiple chemical entities combined through several orthogonal synthesis methods on the interface. Surface chemical modification relies on the use of organoalkoxysilanes that must meet the demand of tuned chemical properties; this, in turn, urges for innovative approaches for having an improved, but simple, organic toolbox. Starting from commonly available molecular precursors, several approaches have emerged: hydrosilylation, click thiol-ene additions, the use of carbodiimides or the reaction between cyclic anhydrides and anchored amines. In this review, we analyze the importance of the COOH groups in the area of materials science and the commercial availability of COOH-based silanes and present new approaches for obtaining COOH-based organoalkoxide precursors. Undoubtedly, this will attract widespread interest for the ultimate design of highly integrated chemical platforms.

The Impact of Different Surface Treatments on Topography and Bond Strength of Resin Cement to Lithium Disilicate Glass Ceramic.

OBJECTIVE: To evaluate the influence of different surface treatments on topography, surface roughness, surface energy, and microtensile bond strength stability of resin cement to lithium disilicate glass ceramic. METHODS AND MATERIALS: Seventy disc-shaped specimens of IPS e.max Press were divided into seven groups according to the surface treatment: NT - non-treated (control); FSil - hydrofluoric acid (HF) + silane; FPSil - HF + phosphoric acid (HP) + silane; FUSil - HF + ultrasonic bath (U) + silane; FPUSil - HF + HP + U + silane; MEP - Monobond Etch and Prime (MEP); and MEPH - MEP + heating. Topography and surface roughness were evaluated using a 3D laser confocal microscope (3DLCM) and scanning electron microscopy (SEM) and surface energy with a goniometer. The microtensile bond strength (µTBS) was evaluated after storage in distilled water at 37°C for 24 hours and after thermocycling (5,000 cycles, 5°-55° C, 30-second dwell time). Data were analyzed using one-way ANOVA (surface roughness and surface energy), two-way ANOVA (µTBS), Tukey's HSD post-hoc test, and Student t-test (α=0.05). RESULTS: FUSil, FPSil, and FSil presented similar and highest surface roughness, whereas NT, FPUSil, MEP, and MEPH showed similar, and lowest, roughness values (p<0.05). FPUSil, FPSil, FUSil, and FSil presented a similar and highest surface energy. NT, MEP, and MEPH showed similar and lowest surface energy. CONCLUSION: Only FSil, FPSil, and MEPH maintained bond strength stability after thermocycling, with FPSil leading to less bond strength reduction, suggesting this protocol is more reliable for bonding resin cements to lithium disilicate glass ceramics.

Evaluation of the Combination of CO2 Laser and Bifunctional Bonding Agents for Composite Resin Repairs After 1 Year of Aging.

Objective: to evaluate the bond strength of repairs to composite resin restorations treated with CO2 laser and bifunctional monomers after 1 year of aging. Background: Adequate bond strength between a composite restoration and resin repair agent can be achieved through mechanical and/or chemical treatment. However, the longevity of such repairs is unknown. Methods: Resin blocks (volume: 125 mm3) were created. Failure surfaces were either not treated or were treated before the repair with a universal adhesive, a silane bonding agent and/or CO2 laser. The blocks were distributed into six groups (n = 6 per group): resin+resin group (RRG), universal adhesive+resin group (ARG), silane+universal adhesive group (SAG), laser+silane+universal adhesive group (LSAG), laser+universal adhesive group (LAG), and laser+silane group (LSG). After treatment, repairs were made with another resin composite. "Sticks" (1.0 mm2 in area and 1.0 cm in length) were cut from the specimens in each group and immersed in distilled water at 37°C. Microtensile bond strength was evaluated after 1 year of aging. Bond strength values were compared using the Kruskal-Wallis test and Dunn's test. Results: Bond strength was significantly higher in the LSAG compared with the RRG, adhesive system, LSG, whereas statistically similar results were found for the SAG, LSAG, and LAG. Bond strength was lowest in the RRG. The LSAG and LAG presented predominantly cohesive fractures. Conclusions: The bond strength of composite resin repairs was satisfactory over time. Treatment with CO2 laser contributed to the maintenance of bond strength during the 1-year storage period and bifunctional monomers present in the universal adhesive on the irradiated repair surface were of fundamental importance to the maintenance of bond strength values, as demonstrated by microtensile bond test and fracture pattern analysis.

Influence of Fit-checking Material and Cleaning Protocols on the Bond Strength of Lithium Disilicate Glass-ceramics.

OBJECTIVES: To evaluate the bond strength of a resin luting agent to a lithium disilicate glass-ceramic after the use of different fit-checking materials and cleaning protocols. METHODS AND MATERIALS: Two hundred and forty-two (242) ceramic specimens were etched with 5% hydrofluoric acid for 20 seconds and distributed into 22 groups (n=10), in total. Four (4) groups were created based on fit-checking material and that had no following cleaning protocol: no fit-checking material used (control group); articulating paper; articulating spray; and fit-checker liquid. For each fit-checking material (3), 6 cleaning protocols were tested creating an additional 18 groups (n=10): air/water spray; 70% alcohol (ethanol); acetone; 35% phosphoric acid; 5% hydrofluoric acid; and a commercially available cleaning paste (Ivoclean, Ivoclar Vivadent). Silane and bonding resin were applied to all ceramic surfaces. Resin luting agent cylinders (1 mm in diameter) were created using silicone matrices, light-cured, and specimens were stored in deionized water at 37°C for 24 hours. Microshear bond strength test (µSBS) was performed on a universal testing machine (DL 500, EMIC) at a crosshead speed of 1 mm/min until failure. Results were statistically analyzed using ANOVA and Tukey's test (α=0.05). RESULTS: Articulating paper and fit-checker liquid, when not properly removed, negatively affected the bond strength (p<0.05). None of the tested cleaning protocols were effective for articulating paper (p<0.05). There was no significant difference in bond strength after the cleaning protocols between articulating spray and fit-checker liquid when compared to the control group (no contamination) (p>0.05). CONCLUSION: The cleaning protocols tested can effectively restore the bond strength of resin luting agents to lithium disilicate ceramics that were exposed to articulating spray or fit-checker liquid. The use of articulating paper is not recommended for fit-checking indirect lithium disilicate restorations.

Biaxial flexure strength and physicochemical characterization of a CAD/CAM lithium disilicate ceramic: effect of etching time, silane, and adhesive applications.

OBJECTIVE: To evaluate the effect of different acid etching time and bonding agent (silane and/or adhesive system) on biaxial flexural strength and physico-chemical properties of a lithium disilicate ceramic. MATERIAL AND METHODS: One hundred twenty ceramic discs were made and divided into 8 groups (n = 15) according to factors "etching time" (20 and 120 s) with hydrofluoric acid (HF) and "bonding agent" (C, no bonding agent; S, silane, A, adhesive; and SA, silane + adhesive). After surface treatment, a resin cement layer was applied to the surface and all specimens were subjected to biaxial flexural strength (BFS) test with treated surfaces loaded in tension (1 mm/min). The Weibull analyses and complementary analyses were also performed. Statistical analysis was done with 2-way ANOVA and the Tukey test (α = 0.05). RESULTS: ANOVA revealed that the factors "etching time" (p = 0.0003) and "bonding agent" (p = 0.007) were statistically significant. In the overall analysis, the HF120S group (272.02 ± 35.30A MPa) presented significantly higher BFS than that of HF120C (218.45 ± 17.15CD MPa) and HF20S (228.40 ± 37.83BCDMPa). On the other hand, the HF20A group (208.92 ± 31.16D MPa) had significantly lower BFS than HF120S (272.02 ± 35.30A), HF120A (254.42 ± 26.87ABC) and HF120SA (259.30 ± 36.55AB) groups (Tukey). The Weibull modulus (m) of all groups was significantly different from each other (p = 0.000). CONCLUSIONS: Regardless of etching time, the application of silane alone is sufficient to increase the flexural strength of glass ceramic, eliminating the need for the application of adhesive systems. Moreover, if only silane or adhesive is applied, 120-s HF application should increase the flexural resistance of the lithium disilicate ceramic. CLINICAL SIGNIFICANCE: Applications of adhesive systems after silanization can be suppressed from the surface treatment protocol of glass ceramics, since it does not improve their mechanical strength.

Push-out Bond Strength of Two Fiber Posts in Composite Resin Using Different Types of Silanization.

OBJECTIVES: The aim of this study was to evaluate the effect of different surface treatments and thermocycling (TC) on the push-out bond strength of two brands of glass fiber posts (GFPs) to composite resin. METHODS: White Post DC (WP) (FGM Dental Group International, Joinville, Santa Catarina, BR) and Exacto (EC) (Angelus, Clinical Research Dental, Londrina, PR, Brazil). GFPs were cleaned with 70% alcohol and divided into five groups, according to the surface treatment (n=15): control (C), without treatment; prehydrolyzed silane (S-pre) (Prosil, FGM Dental Group International); 37% phosphoric acid + prehydrolyzed silane (AcS-pre); Scotchbond Universal Adhesive System (AdU), 3M Oral Care; two-bottle silane (S2B) (Dentsply Sirona Inc). The composite resin was inserted around the posts by using a split matrix. The samples were cut into 1-mm slices. Half of the samples were subjected to the push-out test immediately, and the other half underwent TC before the test. After failure analysis, the data were submitted to three-way analysis of variance (ANOVA) (α=0.05). RESULTS: EC achieved higher bond strength than WP, regardless of TC (p<0.05). Regarding WP, surface treatments (p<0.001) and TC (p<0.001) influenced bonding strength. As for EC without TC, the highest bond strength (p<0.05) was found for C, then AcSpre, S-pre, AdU, and S2B. Application of TC resulted in a statistically higher bond strength values for the EC AcS-pre group (p<0.05), followed by S2B, S-pre, C, and AdU. The WP failures were predominantly cohesive, similar to the EC AdU and EC S2B groups. The other EC groups showed mostly mixed failures. CONCLUSIONS: Surface treatment and TC affected the bond strength to composite resin, depending on which post was used. It is important for dentists to understand the effects of different types of silanization on their chosen post.

Surface Treatment and Cementation of Lithium Silicate Ceramics Containing ZrO2.

OBJECTIVE: To evaluate the effect of different surface treatments on the shear bond strength (SBS) of lithium silicate (LS) and lithium disilicate (LD) ceramics, after thermocycling. METHODS AND MATERIALS: For SBS test, 72 ceramic blocks (18×14×2 mm) were made (24 blocks from each ceramic material): VITA Suprinity (LSS), Celtra Duo (LSC), and Lithium disilicate (LD). The blocks were polished with sandpaper of increasing grit (#280, #400, #800, and #1200) and embedded in chemically activated acrylic resin. Afterwards, they were randomly divided into 12 groups (6 blocks per group) according to: "Ceramic" (LD, LSC, and LSS) and "Surface treatment" (HFS: hydrofluoric acid + silane; MEP: Monobond Etch & Prime/Ivoclar). From each treated surface ceramic block, four dual-curing resin cement cylinders (RelyX U200, 3M Oral Care) were prepared using a Tygon tube (Ø=3 mm and h=2 mm) and light cured for 40 seconds (1000 mW/cm2) (N=288/n=24). All specimens were submitted to thermocycling (10,000 cycles, 5°C and 55°C, 30 seconds) and then to SBS test at a crosshead speed of 1 mm/min using a 50-kgf load cell. Forty-five additional blocks were made for roughness and SEM analysis. Failure mode was also performed. The data (MPa) were statistically analyzed by oneway analysis of variance (ANOVA), Tukey test (5%), and Weibull analysis. The Ra was analyzed by Kruskal-Wallis and Dunn Test (5%). The other variables were analyzed qualitatively. RESULTS: ANOVA revealed that "surface treatment" was significant for all ceramic materials (p<0.05). The LD-HFS (18.66±3.49), LSC-HFS (16.81±2.62), and LSS-HFS (16.33±3.08) groups had significantly higher SBS than the LD-MEP (7.00±4.2), LSCMEP (14.12±3.51), and LSS-MEP (13.87±2.52) groups. Complete adhesive failures at the cement-dentin interface were more frequent. Weibull modulus was superior for the LD-HFS (6.22), LSC-HFS (8.8), and LSS-HFS (7.4) groups. CONCLUSION: HF followed by silanization is the most suitable surface treatment for the cementation of LS and LD glass ceramics.

Antitumor activity of solamargine in mouse melanoma model: relevance to clinical safety.

Melanoma is the most aggressive type of skin cancer, and thus it is important to develop new drugs for its treatment. The present study aimed to examine the antitumor effects of solamargine a major alkaloid heteroside present in Solanum lycocarpum fruit. In addition solamargine was incorporated into nanoparticles (NP) of yttrium vanadate functionalized with 3-chloropropyltrimethoxysilane (YVO4:Eu3+:CPTES:SM) to determine antitumor activity. The anti-melanoma assessment was performed using a syngeneic mouse melanoma model B16F10 cell line. In addition, systemic toxicity, nephrotoxic, and genotoxic parameters were assessed. Solamargine, at doses of 5 or 10 mg/kg/day administered subcutaneously to male C57BL/6 mice for 5 days, decreased tumor size and frequency of mitoses in tumor tissue, indicative of a decrease in cell proliferation. Treatments with YVO4:Eu3+:CPTES:SM significantly reduced the number of mitoses in tumor tissue, associated with no change in tumor size. There were no apparent signs of systemic toxicity, nephrotoxicity, and genotoxicity initiated by treatments either with solamargine alone or plant alkaloid incorporated into NP. The animals treated with YVO4:Eu3+:CPTES:SM exhibited significant increase in spleen weight accompanied by no apparent histological changes in all tissues examined. In addition, animals treated with solamargine (10 mg/kg/day) and YVO4:Eu3+:CPTES:SM demonstrated significant reduction in hepatic DNA damage which was induced by tumor growth. Therefore, data suggest that solamargine may be considered a promising candidate in cancer therapy with no apparent toxic effects.

Non-thermal plasma for surface treatment of inorganic fillers added to resin-based cements.

OBJECTIVES: This study aims to evaluate the effect of non-thermal plasma (NTP) surface treatment in two composite inorganic fillers and evaluate their impact on the chemical-mechanical properties and bond strength ability of experimental resin cements. MATERIALS AND METHODS: Ytterbium fluoride (YF) and barium silicate glass (BS) were characterized and submitted to different surface treatments: non-thermal plasma (NTP); non-thermal plasma and 3-(trimethoxysilyl) propyl methacrylate silanization; and 3-(trimethoxysilyl) propyl methacrylate silanization. Untreated fillers were used as a control. The fillers were incorporated at 65wt% concentration into light-cured experimental resin cements (50wt% BisGMA; 25wt% UDMA; 25wt% TEGDMA; 1mol% CQ). The degree of conversion, the flexural strength, and the microshear bond strength (µSBS) were evaluated to characterize developed composites. RESULTS: YF and BS were successfully cleaned with NTP treatment. Nor NTP neither the silanization affected the degree of conversion of resin cements. The NTP predicted an increase in YF-containing resin cements flexural strength, reducing the storage impact in these materials. NTP treatment did not affect the µSBS when applied to YF, while silanization was effective for BS-containing materials. CONCLUSION: NTP treatment of inorganic particles was possible and was shown to reduce the amount of organic contamination of the particle surface. YF surface treatment with NTP can be an alternative to improve the organic/inorganic interaction in resin composites to obtain materials with better mechanical properties. CLINICAL RELEVANCE: Surface cleaning with NTP may be an alternative for particle surface cleaning to enhance organic-inorganic interaction in dental composites resulting in improved mechanical strength of experimental resin cements.

Antioxidant Activity of Bioactive Peptide Fractions from Germinated Soybeans Conjugated to Fe3O4 Nanoparticles by the Ugi Multicomponent Reaction.

The conjugation of biomolecules to magnetic nanoparticles has emerged as promising approach in biomedicine as the treatment of several diseases, such as cancer. In this study, conjugation of bioactive peptide fractions from germinated soybeans to magnetite nanoparticles was achieved. Different fractions of germinated soybean peptides (>10 kDa and 5-10 kDa) were for the first time conjugated to previously coated magnetite nanoparticles (with 3-aminopropyltriethoxysilane (APTES) and sodium citrate) by the Ugi four-component reaction. The crystallinity of the nanoparticles was corroborated by X-ray diffraction, while the particle size was determined by scanning transmission electron microscopy. The analyses were carried out using infrared and ultraviolet-visible spectroscopy, dynamic light scattering, and thermogravimetry, which confirmed the coating and functionalization of the magnetite nanoparticles and conjugation of different peptide fractions on their surfaces. The antioxidant activity of the conjugates was determined by the reducing power and hydroxyl radical scavenging activity. The nanoparticles synthesized represent promising materials, as they have found applications in bionanotechnology for enhanced treatment of diseases, such as cancer, due to a higher antioxidant capacity than that of fractions without conjugation. The highest antioxidant capacity was observed for a >10 kDa peptide fraction conjugated to the magnetite nanoparticles coated with APTES.

Immobilization of endoglucanase on kaolin by adsorption and covalent bonding.

In the current research, endoglucanase, one of the enzymes of the cellulolytic complex, was immobilized on kaolin by two different techniques, adsorption, and covalent bonding. A comparative study was conducted between free, adsorbed, and covalently immobilized endoglucanase. For the covalent bonding, the kaolin particles were functionalized with 3-aminopropyltriethoxysilane (APTES) and activated with glutaraldehyde. Immobilization by adsorption was performed using the kaolin without any treatment. Recovered activities after the endoglucanase immobilization by adsorption and covalent bonding were found to be 60 ± 2.5 and 65 ± 3.5%, respectively. The studies of optima pH and temperature, as well as thermal stability, showed that the catalytic characteristic of the enzyme was maintained after the immobilization by both adsorption and covalent bonding. Even after 8 cycles of use, the endoglucanase immobilized by the two techniques retained about 86% of its initial activity. The results showed that the adsorption was as effective as covalent bonding for the immobilization of endoglucanase on kaolin. However, the adsorption technique seems to have a greater potential for use in future studies, as it is simpler, cheaper, and faster than covalent immobilization. Therefore, in this work it was demonstrated that endoglucanases can be immobilized efficiently on kaolin through a very simple immobilization protocol, offering a promising strategy for performing repeated enzymatic hydrolysis reactions.

An Approach to the Use of Glycol Alkoxysilane-Polysaccharide Hybrids in the Conservation of Historical Building Stones.

Stone consolidants have been widely used to protect historical monuments. Consolidants and hydrophobic formulations based on the use of tetraethoxysilane (TEOS) and alkylalkoxysilanes as precursors have been widely applied, despite their lack of solubility in water and requirement to be applied in organic media. In the search for a "greener" alternative based on silicon that has potential use in this field, the use of tetrakis(2-hydroxyethyl)silane (THEOS) and tris(2-hydroxyethyl)methyl silane (MeTHEOS) as precursors, due their high water solubility and stability, is proposed in this paper. It is already known that THEOS and MeTHEOS possess remarkable compatibility with different natural polysaccharides. The investigated approach uses the water-soluble silanes THEOS-chitosan and MeTHEOS-chitosan as a basis for obtaining hybrid consolidants and hydrophobic formulations for the conservation of siliceous and calcareous stones. In the case of calcareous systems, their incompatibility with alkoxysilanes is known and is expected to be solved by the developed hybrid consolidant. Their application in the conservation of building stones from historical and archeological sites from Guanajuato, México was studied. The evaluation of the consolidant and hydrophobic formulation treatment was mainly conducted by determining the mechanical properties and contact angle measurements with satisfactory results in terms of the performance and compatibility with the studied stones.

Surface functionalized mesoporous silica nanoparticles for intravitreal application of tacrolimus.

Tacrolimus (TAC), a potent immunosuppressive macrolide, has been investigated for ocular diseases due to promising results in the treatment of anterior and posterior segments eye diseases. Mesoporous and functionalized silica nanoparticles show potential as TAC delivery platforms owing to their interesting characteristic as large surface area, uniform pore size distribution, high pore volume, and excellent biocompatibility. The purpose of this study was to incorporate TAC in functionalized silica nanoparticles with 3-aminopropyltriethoxysilane (MSNAPTES) and investigate the safety and biocompatibility of the systems. The MSNAPTES and MSNAPTES TAC nanoparticles were characterized. The in vitro cytotoxicity of MSNAPTES and MSNAPTES load with TAC (MSNAPTES-TAC) in retinal pigment epithelial cells (ARPE-19) was determined, chorioallantoic membrane (CAM) assay model was used to investigate the in vivo biocompatibility, and safety of intravitreal injection was evaluated using clinical examination (assessment of intraocular pressure and indirect fundus ophthalmoscopy), electroretinographic (ERG) and histologic studies in rats' eyes. The elemental analysis (CHN), thermogravimetric (TGA), photon correlation spectroscopy and Fourier transform infrared (FTIR) analysis confirmed the presence of functionalized agent and TAC in the MSNAPTES nanoparticles. TAC loading was estimated at 7% for the MSNAPTES TAC nanoparticles. MSNAPTES and MSNAPTES TAC did not present in vitro cytotoxicity. The drug delivery systems showed good biocompatibility on CAM. No retinal abnormalities, vitreous hemorrhage, neovascularization, retinal detachment, and optic nerve atrophy were observed during the in vivo study. Follow-up ERGs showed no changes in the function of the retina cells after 15 days of intravitreal injection, and histopathologic observations support these findings. In conclusion, MSNAPTES TAC was successfully synthesized, and physicochemical analyses confirmed the presence of TAC in the nanoparticles. In vitro and in vivo studies indicated that MSNAPTES TAC was safe to intravitreal administration. Taking into account the enormous potential of MSNAPTES to carry TAC, this platform could be a promising strategy for TAC ocular drug delivery in the treatment of eye diseases.

Koh group influence on titanium surfaces and pure sol-gel silica for enhanced osteogenic activity.

Although, the excellent level of success of titanium surfaces is based on the literature, there are some biological challenges such as unfavorable metabolic conditions or regions of poor bone quality where greater surface bioactivity is desired. Seeking better performance, we hypothesized that silica-based coating via sol-gel route with immersion in potassium hydroxide basic solution induces acceleration of bone mineralization. This in vitro experimental study coated titanium surfaces with bioactive glass synthesized by route sol-gel via hydrolysis and condensation of chemical alkoxide precursor, tetraethylorthosilicate (TEOS) and/or deposition of chemical compound potassium hydroxide (KOH) to accelerate bone apposition. The generated surfaces titanium(T), titanium with potassium hydroxide deposition (T + KOH), titanium with bioactive glass deposition synthesized by sol-gel route via tetraethylorthosilicate hydrolysis (TEOS), titanium with bioactive glass deposition synthesized by sol-gel route via tetraethylorthosilicate hydrolysis with potassium hydroxide deposition (TEOS + KOH) were characterized by 3D optical profilometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), contact angle by the sessile drop method, x-ray excited photoelectron spectroscopy (XPS) and energy dispersive x-ray spectrometer (EDX). The addition of the KOH group on the pure titanium (T) or bioactive glass (TEOS) surfaces generated a tendency for better results for mineralization. Groups covered with bioactive glass (TEOS, TEOS + KOH) tended to outperform even groups with titanium substrate (T, T + KOH). The addition of both, bioactive glass and KOH, in a single pure titanium substrate yielded the best results for the mineralization process.

Morphological and Structural Properties of Amino-Functionalized Fumed Nanosilica and Its Comparison with Nanoparticles Obtained by Modified Stöber Method.

In industry, silica nanoparticles (NPs) are obtained by the fuming and the precipitation method. Fumed silica NPs are commonly used in the preparation of nanocomposites because they have an extremely low bulk density (160-190 kg/m3), large surface area (50-600 m2/g), and nonporous surface, which promotes strong physical contact between the NPs and the organic phase. Fumed silica has fewer silanol groups (Si-OH) on its surface than the silica prepared by the Stöber method. However, the number of -OH groups on the fumed silica surface can be increased by pretreating them with sodium hydroxide (NaOH) before further surface modification. In this study, the effectiveness of the NaOH pretreatment was evaluated on commercial fumed silica NPs with a surface area of 200 m2/g. The number of surface -OH groups was estimated by potentiometric titration. The pretreated fumed NPs, and the precipitated NPs (prepared by the Stöber method) were modified with 3-aminopropyltriethoxysilane (APTES) to obtain A200S and nSiO2-APTES, respectively. The NPs were characterized using electron dispersive scanning (EDS), scanning electron microscopy (SEM), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD), BET (Brunauer-Emmett-Teller) analysis, and ζ-potential. XRD confirmed the presence of the organo-functional group on the surface of both NPs. After the amino-functionalization, the ζ-potential values of the nSiO2 and A200 changed from -35.5 mV and -14.4 mV to +26.2 mV and +11.76 mV, respectively. Consequently, we have successfully synthesized functionalized NPs with interesting, specific surface area and porosity (pore volume and size), which can be attractive materials for chemical and energy industries.