Bio-functionalized titanium surfaces with modified silk fibroin carrying titanium binding motif to enhance the ossific differentiation of MC3T3-E1.

Silk fibroin (SF) from Bombyx mori has superior properties as both a textile and a biomaterial, and has been used to functionalize the surfaces of various medical inorganic materials including titanium (Ti). In this study, we endowed SF with reversible binding ability to Ti by embedding a titanium binding motif (minTBP-1 and RKLPDA). Artificial SF proteins were first created by conjugating gene cassettes for SF motif (AGSGAG) and minTBP-1 motif with different ratios, which have been shown to bind reversibly to Ti surfaces in quartz crystal microbalance analyses. Based on these results, the functionalized SF (TiBP-SF) containing the designed peptide [TS[(AGSGAG)3 AS]2 RKLPDAS]8 was prepared from the cocoon of transgenic B. mori, which accelerates the ossific differentiation of MC3T3-E1 cells when coated on titanium substrates. Thus, TiBP-SF presents an alternative for endowing the surfaces of titanium materials with osseointegration functionality, which would allow the exploration of potential applications in the medical field.

Effect of the amount of light energy transmitted through CAD/CAM resin block on bonding performance of four types of resin cement adhesive systems.

Resin-ceramic hybrid materials for computer-aided design/computer-aided manufacturing (CAD/CAM resins) have been developed. In this study, the effects of the amount of light energy transmitted through the four types of 1.5-mm-thick CAD/CAM resin blocks on the bond performance of corresponding resin cement adhesive systems consisting of an adhesive and a dual-curable resin cement were examined. The bond strengths of the four types of resin cement adhesive systems decreased with decreasing the amount of light energy transmitted through CAD/CAM resin block, due to a decrease in the light-curable ability of dual-curable resin cements. However, the degradation behavior of the bond strengths was strongly affected by the types of adhesives and initiator systems utilized. The adhesive consisting of a dimethacrylate monomer and redox-initiators enhanced the bonding performance of the dual-curable resin cement more effectively than the adhesive, which consists of a dimethacrylate monomer and photo-initiators or a γ-me thacryloxypropyltrimethoxysilane and a 10-methacryloyloxydecyl dihydrogen phosphate.

Demineralization capacity of commercial 10-methacryloyloxydecyl dihydrogen phosphate-based all-in-one adhesive.

OBJECTIVE: We determined the amounts of calcium salt of 10-methacryloyloxydecyl dihydrogen phosphate (MDP-Ca salt) and dicalcium phosphate dihydride (DCPD) with an amorphous phase developed during the application of commercial MDP-based all-in-one adhesives to enamel and dentin. This is because the demineralization by MDP and following calcium salt formation of MDP may be limited by an ionic bond formation of MDP to hydroxyapaptite in the enamel and dentin and following intermediary layer formation of MDP, since MDP forms a chemically-stable adsorption layer. METHODS: Scotchbond Universal Adhesive, Clearfil Tri-S Bond ND, Clearfil Tri-S Bond ND Quick, G-Bond Plus and our designed MDP-based all-in-one adhesive were used. Enamel and dentin reactant residues of each adhesive were prepared by varying the adhesive application periods: 1, 30 and 60min, and were analyzed using phosphorous-31 nuclear magnetic resonance and X-ray diffraction. RESULTS: Increasing the adhesive application period to enamel and dentin led to the increased amount of MDP-Ca salt in contrast to amorphous DCPD. In the dentin, each adhesive showed a saturated value on the production amount of MDP-Ca salt when the adhesive was applied more than 30min. In contrast, in the enamel, each adhesive showed an intermediate value on the saturated production amount of MDP-Ca salt that the respective adhesive exhibited. This is due to MDP employed demineralizes the enamel and dentin until MDP was completely consumed yielding MDP-Ca salt. CONCLUSION: Commercial MDP-based all-in-one adhesives would not form an intermediary layer of MDP on hydroxyapatite throughout their application period to enamel and dentin. CLINICAL RELEVANCE: The rate of MDP-Ca salt produced by the demineralization of enamel and dentin depends on the components that constitute commercial adhesive more strongly than on the concentrations of MDP and water in the respective adhesive. This is because HEMA-containing adhesive shows a slower production rate of MDP-Ca salt than HEMA-free adhesive in the enamel and dentin samples.

Effect of the demineralisation efficacy of MDP utilized on the bonding performance of MDP-based all-in-one adhesives.

OBJECTIVES: The amounts of calcium salt of 10-methacryloyloxydecyl dihydrogen phosphate (MDP-Ca salt) and dicalcium phosphate dihydride (DCPD) with an amorphous phase produced by the demineralisation of enamel and dentin were determined using commercial MDP-based 2-hydroxyethyl methacrylate (HEMA)-containing and HEMA-free all-in-one adhesives. The effect of the amount of MDP-Ca salt produced on bonding performance to enamel and dentin was then characterized. METHODS: Three types of commercial HEMA-containing adhesives (Scotchbond Universal Adhesive, Clearfil Tri-S Bond ND, Clearfil Tri-S Bond ND Quick), a commercial HEMA-free adhesive (G-Bond Plus) and an experimental HEMA-free adhesive were used. The reactant residues of each adhesive were prepared after interacting with enamel and dentin samples for 60 s. The amounts of MDP-Ca salt and amorphous DCPD produced were determined using a phosphorous-31 nuclear magnetic resonance technique. Enamel and dentin bond strengths were measured for each adhesive, with and without thermocycling. RESULTS: The amounts of MDP-Ca salt and amorphous DCPD formed after interacting with enamel and dentin differed among the five adhesives and were independent of their pH values. Enamel showed a strong positive-correlation of the bond strength of the all-in-one adhesives to the amount of MDP-Ca salt produced, however, the dentin showed a weak negative-correlation. CONCLUSION: The HEMA-free all-in-one adhesives showed a greater efficacy to demineralise the enamel and dentin than the HEMA-containing all-in-one adhesives. The dentin showed a different effect of the amount of MDP-Ca salt produced on the bonding performance compared with enamel. CLINICAL SIGNIFICANCE: The enamel bond strength of MDP-based all-in-one adhesives strongly contributes to the demineralisation efficacy by the incorporation of MDP, in contrast to the dentin bond strength. However, the efficacy of MDP-based all-in-one adhesives to demineralise the enamel and dentin is not directly related to the pH value of the MDP-based all-in-one adhesive.

NMR study on the demineralization mechanism of the enamel and dentin surfaces in MDP-based all-in-one adhesive.

The acidic monomers utilized in all-in-one adhesives play a key role in the enamel and dentin bonding performance. The purpose of this study is to investigate the mechanism by which 10-methacryloyloxydecyl dihydrogen phosphate (MDP) demineralizes the enamel and dentin surfaces prepared by a diamond bur in three types of experimental MDP-based all-in-one (EX) adhesives containing different amounts of water (46.6, 93.2 and 208.1 mg/g). The enamel and dentin reactants of EX adhesives were analyzed using solidstate phosphorous-31 nuclear magnetic resonance and X-ray diffraction. Increased amount of water led to increases in the efficacy by which MDP demineralizes the enamel and dentin surfaces. However, the rate of calcium salts of MDP produced slowed down at the water concentrations above 93.2 mg/g. The dentin yielded greater amounts of di-calcium salts of the MDP monomer and dimer than the enamel, which develops a different type of layered structure of MDP from the enamel.

Glass fiber-reinforced thermoplastics for use in metal-free removable partial dentures: combined effects of fiber loading and pigmentation on color differences and flexural properties.

PURPOSE: The purpose of this study was to investigate the combined effects of fiber loading and pigmentation on the color differences and flexural properties of glass fiber-reinforced thermoplastics (GFRTPs), for use in non-metal clasp dentures (NMCDs). METHODS: The GFRTPs consisted mainly of E-glass fibers, a polypropylene matrix, and a coloring pigment: the GFRTPs with various fiber loadings (0, 10, and 20mass%) and pigmentations (0, 1, 2, and 4mass%) were fabricated by using an injection molding. The color differences of GFRTPs were measured based on the Commission Internationale de l'Eclairage (CIE) Lab color system, by comparing with a commercially available NMCD. The flexural properties of GFRTPs were evaluated by using a three-point bending test, according to International Standards Organization (ISO) specification number 20795-1. RESULTS: The visible colors of GFRTPs with pigment contents of 2mass% were acceptable for gingival color, and the glass fibers harmonized well with the resins. The ΔE* values of the GFRTPs with pigment contents of 2mass% obtained by using the CIE Lab system were lowest at all fiber loadings. For GFRTPs with fiber contents of 10 and 20mass% at 2mass% pigment content, these GFRTPs surpassed the ISO 20795-1 specification regarding flexural strength (> 60MPa) and modulus (> 1.5GPa). CONCLUSIONS: A combination of the results of color difference evaluation and mechanical examination indicates that the GFRTPs with fiber contents of 10 or 20mass%, and with pigment contents of 2mass% have acceptable esthetic appearance and sufficient rigidity for NMCDs.

Color stability of glass-fiber-reinforced polypropylene for non-metal clasp dentures.

PURPOSE: The purpose of this study was to investigate the color stability of a glass-fiber-reinforced thermoplastic (GFRTP), for use in non-metal clasp dentures (NMCDs). METHODS: GFRTPs composed of E-glass fibers and polypropylene with 2 mass% of pigments were fabricated using injection molding. According to our previous study on the optimum fiber content for GFRTPs, we prepared GFRTPs with fiber contents of 0, 10, and 20 mass% (GF0, GF10, and GF20). Commercially available NMCD and PMMA materials were used as controls. The color changes of GFRTPs at 24h, and at 1, 2, and 4 weeks of coffee immersion at 37°C were measured by colorimetry, using the Commission Internationale de l'Eclairage (CIE) Lab system. The color stabilities of the GFRTPs were evaluated in two units: the color difference (ΔE∗) and National Bureau of Standards (NBS) units. RESULTS: After immersion, none of the GFRTPs showed visible color change. From the colorimetry measurement using the CIE Lab system, the ΔE∗ values of the GFRTPs were 0.65-2.45. The NBS values of the GFRTPs were 0.60-2.25, all lower than the threshold level of 3.0, demonstrating clinically acceptable color changes. On the other hand, an available polyamide-based NMCD material exhibited "appreciable" color change, as measured in NBS units. CONCLUSIONS: The results indicate that the GFRTPs showed clinically acceptable color stability and might be satisfactory for clinical use. Therefore, GFRTPs are expected to become attractive materials for esthetic dentures.

Zirconia surface modification by a novel zirconia bonding system and its adhesion mechanism.

OBJECTIVE: Bonding to zirconia has been of great interest over the last 10-15 years. The aim of this study was to develop a zirconia bonding system and clarify its adhesion mechanism. METHODS: A zirconia primer was prepared using tetra-n-propoxy zirconium (TPZr) and water. A silane primer was also prepared using γ-methacryloyloxypropyltrimethoxysilane (γ-MPS) and hydrochloric acid. After the zirconia primer was applied to the oxidized zirconia surface, the silane primer was applied to the ZrO2-functionalized layer and the resin cement was applied to the silane-modified layer. Ceramic Primer II was used as a typical MDP-based ceramic primer. Shear bond strengths were measured using a universal testing machine. To clarify the enhancing mechanism of the zirconia bonding system, X-ray photoelectron spectroscopy (XPS) analyses were performed. RESULTS: The zirconia bond strength was affected by the surface wettability of zirconia, and the compositions of TPZr and water utilized in the zirconia primer. When the zirconia primer, consisting of 10µL TPZr and 13µL water, was applied to the zirconia surface that had been oxidized by H2O2 above 10%, the maximum bond strength of 8.2MPa was obtained. The mechanism of the zirconia bonding system was established as follows: the hydrolyzed zirconium species formed a more reactive ZrO2-functionalized layer on the oxidized zirconia surface, and the hydrolyzed γ-MPS species adsorbed on that layer introduces a chemical bonding to the resin. SIGNIFICANCE: The novel zirconia bonding system enhanced the bonding performance of the resin, and showed a greater bond strength than an MDP-based ceramic primer.

Effect of fiber content on flexural properties of glass fiber-reinforced polyamide-6 prepared by injection molding.

The use of non-metal clasp denture (NMCD) materials may seriously affect the remaining tissues because of the low rigidity of NMCD materials such as polyamides. The purpose of this study was to develop a high-rigidity glass fiber-reinforced thermoplastic (GFRTP) composed of E-glass fiber and polyamide-6 for NMCDs using an injection molding. The reinforcing effects of fiber on the flexural properties of GFRTPs were investigated using glass fiber content ranging from 0 to 50 mass%. Three-point bending tests indicated that the flexural strength and elastic modulus of a GFRTP with a fiber content of 50 mass% were 5.4 and 4.7 times higher than those of unreinforced polyamide-6, respectively. The result showed that the physical characteristics of GFRTPs were greatly improved by increasing the fiber content, and the beneficial effects of fiber reinforcement were evident. The findings suggest that the injection-molded GFRTPs are adaptable to NMCDs because of their excellent mechanical properties.

Fabrication and physical properties of glass-fiber-reinforced thermoplastics for non-metal-clasp dentures.

Recently, non-metal-clasp dentures (NMCDs) made from thermoplastic resins such as polyamide, polyester, polycarbonate, and polypropylene have been used as removable partial dentures (RPDs). However, the use of such RPDs can seriously affect various tissues because of their low rigidity. In this study, we fabricated high-rigidity glass-fiber-reinforced thermoplastics (GFRTPs) for use in RPDs, and examined their physical properties such as apparent density, dynamic hardness, and flexural properties. GFRTPs made from E-glass fibers and polypropylene were fabricated using an injection-molding. The effects of the fiber content on the GFRTP properties were examined using glass-fiber contents of 0, 5, 10, 20, 30, 40, and 50 mass%. Commercially available denture base materials and NMCD materials were used as controls. The experimental densities of GFRTPs with various fiber contents agreed with the theoretical densities. Dynamic micro-indentation tests confirmed that the fiber content does not affect the GFRTP surface properties such as dynamic hardness and elastic modulus, because most of the reinforcing glass fibers are embedded in the polypropylene. The flexural strength increased from 55.8 to 217.6 MPa with increasing glass-fiber content from 0 to 50 mass%. The flexural modulus increased from 1.75 to 7.42 GPa with increasing glass-fiber content from 0 to 50 mass%, that is, the flexural strength and modulus of GFRTP with a fiber content of 50 mass% were 3.9 and 4.2 times, respectively, those of unreinforced polypropylene. These results suggest that fiber reinforcement has beneficial effects, and GFRTPs can be used in NMCDs because their physical properties are better than those of controls. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 2254-2260, 2017.

Effect of the surface morphology of silk fibroin scaffolds for bone regeneration.

Existing scaffolds cannot adequately satisfy the simultaneous requirements for the regeneration of bone. The challenge remains of how to improve the integration of newly formed bone with the surrounding tissues. The purpose of this study was to investigate the effects of two silk fibroin scaffolds, a hexafluoro isopropanol-based silk fibroin (HFIP-F) and an aqueous-based silk fibroin (A-F), for their osteoinductive potentials in large critical size bone defects in vivo. ß-tricalcium phosphate (ß-TCP) was used as a positive control. After implantation into defects created in the knee joints of rabbits for 1 and 2 weeks, hematoxylin and eosin (H-E) and Azan staining revealed that the A-F scaffold as well as ß-TCP had stronger osteoinductive ability than the HFIP-F scaffold. The A-F scaffold exhibited prominent areas of neo-tissue containing bone-like nodules. Furthermore, induced osteointegration was observed between native and neo-tissue within the osteo defects in the knee joints of rabbits. Immunohistochemical staining showed the highest expression of Runx2, BMP-2, BMP-7, Smad1/5/9 and Phospho-Smad in the A-F scaffold implants. Osteoinduction of the porous A-F scaffold might be influenced by the amount of BMP signaling present in the local microenvironment in the implants. This study opens a new avenue to use A-F silk fibroin scaffolds for the regeneration of bone defects.

Quantitative Evaluation of MDP-Ca Salt and DCPD after Application of an MDP-based One-step Self-etching Adhesive on Enamel and Dentin.

PURPOSE: To investigate the effects of an experimental 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based one-step self-etching adhesive (EX adhesive) applied to enamel and dentin on the production of calcium salt of MDP (MDP-Ca salt) and dicalcium phosphate dehydrate (DCPD) at various periods. MATERIALS AND METHODS: The EX adhesive was prepared. Bovine enamel and dentin reactants were prepared by varying the application period of the EX adhesive: 0.5, 1, 5, 30, 60 and 1440 min. Enamel and dentin reactants were analyzed using x-ray diffraction and solid-state phosphorus-31 nuclear magnetic resonance (31P NMR). Curvefitting analyses of corresponding 31P NMR spectra were performed. RESULTS: Enamel and dentin developed several types of MDP-Ca salts and DCPDs with amorphous and crystalline phases throughout the application period. The predominant molecular species of MDP-Ca salt was determined as the monocalcium salt of the MDP monomer. Dentin showed a faster production rate and greater produced amounts of MDP-Ca salt than did enamel, since enamel showed a knee-point in the production rate of the MDP-Ca salt at the application period of 5 min. In contrast, enamel developed greater amounts of DCPD than did dentin and two types of DCPDs with different crystalline phases at application periods > 30 min. The amounts of MDP-Ca salt developed during the 30-s application of the EX adhesive on enamel and dentin were 7.3 times and 21.2 times greater than DCPD, respectively. CONCLUSION: The MDP-based one-step adhesive yielded several types of MDP-Ca salts and DCPD with an amorphous phase during the 30-s application period on enamel and dentin.

Surface topography, hardness, and frictional properties of GFRP for esthetic orthodontic wires.

In our previous study, glass-fiber-reinforced plastics (GFRPs) made from polycarbonate and glass fiber for esthetic orthodontic wires were prepared by using pultrusion. The purpose of the present study was to investigate the surface topography, hardness, and frictional properties of GFRPs. To investigate how fiber diameter affects surface properties, GFRP round wires with a diameter of 0.45 mm (0.018 in.) were prepared incorporating either 13 µm (GFRP-13) or 7 µm (GFRP-7) glass fibers. As controls, stainless steel (SS), cobalt-chromium-nickel alloy, ß-titanium (ß-Ti) alloy, and nickel-titanium (Ni-Ti) alloy were also evaluated. Under scanning electron microscopy and scanning probe microscopy, the ß-Ti samples exhibited greater surface roughness than the other metallic wires and the GFRP wires. The dynamic hardness and elastic modulus of GFRP wires obtained by the dynamic micro-indentation method were much lower than those of metallic wires (p < 0.05). Frictional forces against the polymeric composite brackets of GFRP-13 and GFRP-7 were 3.45 ± 0.49 and 3.60 ± 0.38 N, respectively; frictional forces against the ceramic brackets of GFRP-13 and GFRP-7 were 3.39 ± 0.58 and 3.87 ± 0.48 N, respectively. For both bracket types, frictional forces of GFRP wires and Ni-Ti wire were nearly half as low as those of SS, Co-Cr, and ß-Ti wires. In conclusion, there was no significant difference in surface properties between GFRP-13 and GFRP-7; presumably because both share the same polycarbonate matrix. We expect that GFRP wires will deliver superior sliding mechanics with low frictional resistance between the wire and bracket during orthodontic treatment.

Determination of molecular species of calcium salts of MDP produced through decalcification of enamel and dentin by MDP-based one-step adhesive.

Enamel and dentin particles were added to an experimental 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based one-step adhesive to react for 30 s. After enamel and dentin reactants were analyzed using X-ray diffraction (XRD) and phosphorus-31 nuclear magnetic resonance ((31)P NMR) techniques, curve-fitting analysis was performed on the (31)P NMR spectra of enamel and dentin reactants. By varying the molar ratio of calcium chloride to MDP, a series of three types of MDP-Ca salts were synthesized. The molecular species of calcium salts of MDP (MDP-Ca salts) produced by decalcification of enamel or dentin were determined based on the XRD and (31)P NMR analysis results of these three types of synthesized MDP-Ca salts. Curve-fitting analysis showed that enamel and dentin developed several types of MDP-Ca salts and amorphous dicalcium phosphate dihydrate (DCPD) during decalcification. The molecular species of MDP-Ca salts produced by enamel and dentin were mono-calcium salts of MDP monomer and MDP dimer. In addition, dentin produced a di-calcium of MDP dimer.

Preparation, mechanical, and in vitro properties of glass fiber-reinforced polycarbonate composites for orthodontic application.

Generally, orthodontic treatment uses metallic wires made from stainless steel, cobalt-chromium-nickel alloy, ß-titanium alloy, and nickel-titanium (Ni-Ti) alloy. However, these wires are not esthetically pleasing and may induce allergic or toxic reactions. To correct these issues, in the present study we developed glass-fiber-reinforced plastic (GFRP) orthodontic wires made from polycarbonate and E-glass fiber by using pultrusion. After fabricating these GFRP round wires with a diameter of 0.45 mm (0.018 inch), we examined their mechanical and in vitro properties. To investigate how the glass-fiber diameter affected their physical properties, we prepared GFRP wires of varying diameters (7 and 13 µm). Both the GFRP with 13-µm fibers (GFRP-13) and GFRP with 7 µm fibers (GFRP-7) were more transparent than the metallic orthodontic wires. Flexural strengths of GFRP-13 and GFRP-7 were 690.3 ± 99.2 and 938.1 ± 95.0 MPa, respectively; flexural moduli of GFRP-13 and GFRP-7 were 25.4 ± 4.9 and 34.7 ± 7.7 GPa, respectively. These flexural properties of the GFRP wires were nearly equivalent to those of available Ni-Ti wires. GFRP-7 had better flexural properties than GFRP-13, indicating that the flexural properties of GFRP increase with decreasing fiber diameter. Using thermocycling, we found no significant change in the flexural properties of the GFRPs after 600 or 1,200 cycles. Using a cytotoxicity detection kit, we found that the glass fiber and polycarbonate components comprising the GFRP were not cytotoxic within the limitations of this study. We expect this metal-free GFRP wire composed of polycarbonate and glass fiber to be useful as an esthetically pleasing alternative to current metallic orthodontic wire.

Effects of degree of dissociation of acid used on hydrolytic durability of ceramic primer.

In this study, effects of the degree of dissociation of acids on the hydrolysis rate of methoxy group in γ-methacryloxypropyltrimethoxysilane (γ-MPS) and the adsorption characteristics of γ-MPS on ceramic surfaces were studied using acetic, phosphoric, and hydrochloric acids. Hydrolytic stability of γ-MPS adsorption layer at the resin-ceramic interface was thus examined. (29)Si NMR observations of acidactivated γ-MPS and contact angle measurements following ceramic surface silanization were performed. Bond strengths of resin to the silanized ceramic surfaces were measured. Statistical analyses of shear bond strength and contact angle data were performed. Increase in the degree of dissociation of the acid used increased the hydrolysis rate of methoxy group in γ-MPS, but lowered the contact angle to the silanized ceramic surface. Decrease in the contact angle increased the hydrolytic stability of γ-MPS adsorption layer.

Effect of plasma-irradiated silk fibroin in bone regeneration.

We have recently identified plasma-irradiated silk fibroin (P-AF) as a key regulator of bone matrix properties and composition. Bone matrix properties were tested in 48 femur critical size defects (3.25 mm in diameter) with the expression of osteoblast specific genes at 1 and 2 weeks after surgery. The scaffolds were characterized by various states of techniques; the scanning electronic microcopy revealed the large sized pores in the aqueous-based silk fibroin (A-F) scaffold and showed no alteration into the architecture by the addition of plasma irradiation. The contact angle measurements confirmed the introduction of plasma helped to change the hydrophobic nature into hydrophilic. The histological analyses confirmed the presence of silk fibroin in scaffolds and newly formed bone around the scaffolds. Immunohistochemical examination revealed the increased expression pattern in a set of osteoblast specific genes (TGF-ß, TGF-ß type III receptor, Runx2, type I collagen and osteocalcin). These data were the first to show that the properties of bone matrix are regulated, specifically through Runx2 pathway in P-AF group. Thus, an employment of P-AF increases several compositional properties of bone, including increased bone matrix, mineral concentration, cortical thickness, and trabecular bone volume.

Development of MDP-based one-step self-etch adhesive--effect of additional 4-META on bonding performance.

We designed three experimental 10-methacryloyloxydecyl dihydrogen phosphate (MDP)-based one-step (EX) adhesives consisting of MDP, urethane dimethacrylate, and triethylene glycol dimethacrylate adhesives with different water contents (98.4, 196.8, and 294.4 mg/g), and 4-methacryloyloxyethyl trimellitic anhydride (4-META) or 2-hydroxyethyl methacrylate (HEMA)-containing onestep adhesive. The effect of the amount of MDP-calcium (MDP-Ca) salt produced through demineralization of enamel and dentin on the bonding performance was examined. The efficacy of 4-META and HEMA was then discussed. When the amount of water in EX adhesive was increased, the production amount of MDP-Ca salt of enamel increased, but not the dentin. The enamel bond strength slightly increased with increasing the production amount of MDP-Ca salt, in contrast to the dentin. However, addition of 4-META in the EX adhesive (water content=98.4 mg/g) increased both bond strengths, although the production amounts of MDP-Ca salt significantly decreased. The 4-META enhances both bond strengths more effectively than the HEMA.

Silk fibroin-based scaffolds for bone regeneration.

Porous scaffolds were prepared using regenerated Bombyx mori silk fibroin dissolved in water or hexafluoroisopropanol (HFIP). The effects of these two preparations on the formation and growth of new bone on implantation into the rabbit femoral epicondyle was examined. The aqueous-based fibroin (A-F) scaffold exhibited significantly greater osteoconductivity as judged by bone volume, bone mineral content, and bone mineral density at the implant site than the HFIP-based fibroin (HFIP-F) scaffold. Micro-CT analyses showed that the morphology of the newly formed bone differed significantly in the two types of silk fibroin scaffold. After 4 weeks of implantation, new trabecular bone was seen inside the pores of the A-F scaffold implant while the HFIP-F scaffold only contained necrotic cells. No trabecular bone was seen within the pores of the latter scaffolds, although the pores of these did contain giant cells and granulation tissue.

Ceramic bond durability and degradation mechanism of commercial gamma-methacryloxypropyl trimethoxysilane-based ceramic primers.

PURPOSE: To investigate the bond durability and degradation mechanism of various commercial ceramic primers that are based on gamma-methacryloxypropyl trimethoxysilane (gamma-MPTS) and contain various organic additives. The null hypotheses tested were that (1) the type of ceramic primer had no effect on the bond strength after thermocycling and (2) the type of ceramic primer had no effect on the water contact angle after rinsing with THF. METHODS: The adherent was a silica-based ceramic block used for computer-aided design/computer-aided manufacturing (CAD-CAM). Four commercial ceramic primers, Clearfil Mega Bond Porcelain Bonding kit (CM), Tokuso ceramic primer (TC), GC ceramic primer (CP), and Porcelain Liner M (PL), were compared with a simplified experimental ceramic primer (EP) that comprised gamma-MPTS and an inorganic acid (hydrochloric acid) but no other organic additives. The specimens for the adhesion test were prepared after a dual-curing type resin cement (Link Max) had adhered to the ceramic surfaces treated with each ceramic primer. The bonded specimens were then stored in water at 37 degrees C for 1 day. Then, the bonded specimens were thermocycled between 5 degrees C and 55 degrees C in water baths for 5000 or 10,000 cycles. The dwell time in each water bath and the transfer time were 60 and 7 seconds, respectively. The shear bond strength of resin to the ceramic surface was measured under a crosshead speed of 1.0 mm/minute by a conventional testing machine. Thereafter, the fracture mode for each specimen was determined. In addition, the water contact angle on the treated ceramic surfaces was measured before and after THF using a cotton pellet. As a control, the contact angle on the ground ceramic surface was measured without any ceramic primer. RESULTS: For all samples, thermocycling led to an increase in the frequency of interfacial failure, reflecting reduced mean bond strength of the resin to the treated ceramic surfaces. However, the bond degradation behavior differed among commercial ceramic primers; in particular, PL exhibited different ceramic bond durability from the others. However, the mean bond strength of PL was only 11.8 MPa and over half the specimens exhibited interfacial failure. In contrast, EP provided significantly higher mean bond strength of 17.2 MPa and most specimens exhibited cohesive failure of the ceramic. Furthermore, the contact angle measurements clearly demonstrated that the commercial ceramic primers created a multilayer consisting of gamma-MPTS species and the organic additives on the ceramic surface.