Influence of Oxidative Etching Solution Temperatures on the Surface Roughness and Wettability of a Titanium Alloy.

Recently, a simple surface modification treatment of titanium (Ti) was developed to produce nano-and micro-scale features on the surfaces via simple immersion in an oxidative aqueous solution (30% hydrogen peroxide/5% sodium bicarbonate). However, this treatment method of Ti surfaces requires a relatively long immersion time (4 h) in the oxidative solution. In this study, we investigated whether an increase in the temperature of the oxidative etching solution can shorten the immersion time of Ti effectively. Polished grade 5 dental Ti (Ti-6Al-4V) discs were immersed in the oxidative aqueous solution either for 30 or 60 min. The temperature of the etching solution was maintained at 25 (similar to room temperature), 35, or 45 °C during etching. The etched surfaces were studied in terms of micro- and nano-structures, surface roughness, and wettability (surface energy). The increase in the temperature of the solution accelerated the etching effect of Ti and created both micro- and nano-structures on the surfaces more effectively. In particular, immersion for 60 min at the solution temperature of 35 °C significantly increased the surface roughness and wettability, although the etching effect was enhanced further at the solution temperature of 45 °C.

Antifungal Effect of a Dental Tissue Conditioner Containing Nystatin-Loaded Alginate Microparticles.

In this in vitro study, nystatin-alginate microparticles were successfully fabricated to control the release of nystatin from a commercial dental tissue conditioner. These nystatin-alginate microparticles were spherical and had a slightly rough surface. The microparticles incorporated into the tissue conditioner were distributed homogeneously throughout the tissue conditioner matrix. The incorporation of the microparticles did not deteriorate the mechanical properties of the original material. The agar diffusion test results showed that the tissue conditioner containing the microparticles had a good antifungal effect against Candida albicans. The nystatin-alginate microparticles efficiently controlled the release of nystatin from the tissue conditioner matrix over the experimental period of 14 days. Moreover, the nystatin-alginate microparticles incorporated in the tissue conditioner showed effective antifungal function even at lower concentrations of nystatin. The current study suggests that the tissue conditioner containing the nystatin-alginate microparticle carrier system has potential as an effective antifungal material.

Resin Bonding to Type IV Gold Alloy Conditioned with a Novel Mercapto Silane System: Effect of Incorporation of a Phosphate Monomer.

Self-assembled monolayers of thiols have been used to link a range of materials to planar gold surfaces or gold nanoparticles in nanoscience and nanotechnology. Novel mercapto silane systems are a promising alternative to dental noble metal alloys for enhanced resin bonding durability Goldbased alloys for full-cast restorations contain various base metal elements, which may bond to acidic functional monomers chemically, in addition to noble metal elements. This study examined how the additional incorporation of a phosphate monomer (di-2-hydroxyethyl methacryl hydrogenphosphate, DHP) into novel mercapto silane primer systems affected the resin bond strength to a type IV gold alloy pretreated with the primers. One of three commercial primers (Alloy Primer and M. L. Primer) and three experimental primer systems ((1) blend of γ-mercaptopropyltrimethoxysilane (SPS) and γ-methacryloxypropyltrimethoxysilane (MPS) (both 1.0 wt%), (2) 1.0 wt% DHP-containing primer, and (3) blend of SPS, MPS, and DHP (each 1.0 wt%)) was applied to the alloy surfaces after sandblasting. Resin cylinders (diameter: 2.38 mm) were bonded to the surfaces and light-cured. All bonded specimens were stored in water at 37 °C for 24 h and then half of them additionally water immersed for 7 days (37 °C) and thermocycled 10,000 times before the shear bond strength test (n = 10). The mercapto silane systems (SPS + MPS) were found to show superior resin bonding durability to the commercial primers and the only DHP-containing primer, regardless of additional incorporation of the phosphate monomer.

Synthesis and Characterization of ß-Tricalcium Phosphate Derived From Haliotis sp. Shells.

PURPOSE: To develop a methodology for the synthesis of ß-tricalcium phosphate (ß-TCP, Ca3(PO4)2) from the shell of Haliotis sp. (abalone shell) and to verify its characterization and biocompatibility. MATERIALS AND METHODS: Calcium oxide (CaO) was synthesized from abalone shell by sintering and was suspended in distilled water to prepare calcium hydroxide (Ca(OH)2). For the synthesis of calcium carbonate (CaCO3), carbon dioxide was used to infuse Ca(OH)2 at pH 7.4. CaCO3 was reacted with phosphoric acid at pH 6.0 to obtain dicalcium phosphate (CaHPO4). Subsequently, ß-TCP was synthesized by a chemical reaction between CaHPO4 and CaO at 950°C to 1100°C for 3 hours. Fourier transform infrared spectroscopy (FT-IR) and x-ray diffraction (XRD) was performed to verify the physiochemical characteristics of the composite synthesized from abalone shell. RESULTS: FT-IR and XRD results showed that ß-TCP was successfully synthesized from abalone shell. The synthesized ß-TCP did not affect cell viability of either normal human oral keratinocytes or osteoblastic MG-63 cells. These data indicate that ß-TCP synthesized from abalone shell is biologically safe. CONCLUSIONS: ß-TCP (Ca3(PO4)2) synthesized from abalone shell can be used as a potential source of bone grafting material.

Antimicrobial Activity of Glass lonomer Cement Incorporated with Chlorhexidine-Loaded Zeolite Nanoparticles.

A functional dental restorative system with antimicrobial properties was developed using zeolite (ZE) nanoparticles (NPs) as a drug delivery carrier. ZE NPs loaded with chlorhexidine (CHX) were prepared using the ionic immobilization method. The resulting CHX-loaded ZE NPs were then incorporated into commercial dental glass ionomer cement (GIC). The average size of the CHX-loaded ZE NPs was about 100 to 200 nm, and the NPs were dispersed homogeneously in the GIC. The in vitro release profile of encapsulated GIC containing CHX showed an early release burst of approximately 30% of the total CHX by day 7, whereas GIC containing CHX-loaded ZE NPs showed a sustained release of CHX without the early release burst in a 4-week immersion study. The agar diffusion test results showed that the GIC incorporated with CHX-loaded ZE NPs showed a larger growth inhibition zone of Streptococcus mutans than GIC alone, indicating that this innovative delivery platform potently imparted antimicrobial activity to the GIC. Moreover, these findings suggest that a range of antimicrobial drugs that inhibit the growth of oral bacteria can be incorporated efficiently into dental GIC using CHX-loaded ZE NPs.

Osteogenic Evaluation of Porous Calcium Phosphate Granules with Drug Delivery System Using Nanoparticle Carriers.

Novel porous biphasic calcium phosphate (BCP) granules incorporated with drug-releasing poly(lactic-co-glycolic acid) (PLGA) nanoparticles were developed as a drug delivery platform for bone regeneration. The charge interaction between the BCP and PLGA nanoparticle surfaces was manipulated to create this combination system. Spherical BCP granules with open micro-channels and PLGA nanoparticles loaded with dexamethasone (DEX) as a model drug were fabricated using a liquid nitrogen method and standard emulsion method, respectively. Polyethyleneimine was coated on the DEX-loaded PLGA nanoparticle surfaces, resulting in a net positively charged surface. Such modified nanoparticles were immobilized physically on the negatively charged BCP granule surfaces. An in vitro evaluation of MG 63 cells cultured for 1 and 2 weeks on the BCP granules containing DEX-loaded PLGA nanoparticles showed greater cell proliferation, differentiation, and a more extensively connected-tissue network than those cultured on the BCP granules alone. This innovative platform for bioactive molecule delivery more potently induced osteogenesis in vitro, which might be exploited in implantable bioceramic bone graft materials for stem cell therapy or improved in vivo performance.

Simple Heat Treatment of Zirconia Ceramic Pre-Treated with Silane Primer to Improve Resin Bonding.

Establishing a strong resin bond to dental zirconia ceramic remains difficult. Previous studies have shown that the conventional application of silane does not work well with zirconia. This paper reports that a silane pre-treatment of dental zirconia ceramic combined with subsequent heat treatment has potential as an adhesive cementation protocol for improving zirconia-resin bonding. Among the various concentrations (0.1 to 16 vol%) of experimental γ-methacryloxypropyltrimethoxysilane (γ-MPTS) primers assessed, the 1% solution was found to be the most effective in terms of the shear bond strength of the resin cement to dental zirconia ceramic. A high shear bond strength (approx. 30 MPa) was obtained when zirconia specimens were pre-treated with this primer and then heat-treated in a furnace for 60 min at 150 degrees C. Heat treatment appeared to remove the hydrophilic constituents from the silane film formed on the zirconia ceramic surface and accelerate the condensation reactions between the silanol groups of the hydrolyzed silane molecules at the zirconia/resin interface, finally making a more desirable surface for bonding with resin. This estimation was supported by Fourier transform infrared spectroscopy of the silanes prepared in this study.

The Effect of Novel Mercapto Silane Systems on Resin Bond Strength to Dental Noble Metal Alloys.

Self-assembled monolayers of thiols (RSH), which are key elements in nanoscience and nanotechnology, have been used to link a range of materials to planar gold surfaces or gold nanoparticles. In this study, the adhesive performance of mercapto silane systems to dental noble metal alloys was evaluated in vitro and compared with that of commercial dental primers. Dental gold-palladium-platinum (Au-Pd-Pt), gold-palladium-silver (Au-Pd-Ag), and palladium-silver (Pd-Ag) alloys were used as the bonding substrates after air-abrasion (sandblasting). One of the following primers was applied to each alloy: (1) no primer treatment (control), (2) three commer- cial primers: V-Primer, Metal Primer II, and M.L. Primer, and (3) two experimental silane primer systems: 2-step application with 3-mercaptopropyltrimethoxysilane (SPS) (1.0 wt%) and then 3-methacryloxypropyltrimethoxysilane (MPS) (1.0 wt%), and a silane blend consisting of SPS and MPS (both 1.0 wt%). Composite resin cylinders with a diameter of 2.38 mm were bonded to the surfaces and irradiated for 40 sec using a curing light. After storage in water at 37 °C for 24 h, all the bonded specimens were thermocycled 5000 times before the shear bond strength test. Regardless of the alloy type, the mercapto silane systems (both the 2-step and blend systems) consistently showed superior bonding performance than the commercial primers. Contact angle analysis of the primed surfaces indicated that higher resin bond strengths were produced on more hydrophilic alloy surfaces. These novel mercapto silane systems are a promising alternative for improving resin bonding to dental noble metal alloys.

In Vitro Evaluation of Hydroxyapatite-Coated Titanium Implant with Atmospheric Plasma Treatment.

Plasma treatments are becoming a popular method for modifying the characteristics of a range of substrate surfaces. Atmospheric pressure plasma (APP) is cost-efficient, safe and simple compared to high-pressure plasma. This study examined the effects of a low-temperature APP treatment of a hydroxyapatite (HA)-coated Ti (HA-Ti) surface. The APP treatment made the HA-Ti surfaces more hydrophilic without changing surface morphologies. The APP-treated HA-Ti (APP-HA-Ti) surface showed enhanced cell spreading, cell proliferation, and alkaline phosphatase (ALP) levels with more developed cellular networks, and the formed extracellular matrix (ECM) was fused perfectly with the HA substrate than that on the HA-Ti surface. In conclusion, an APP treatment is a potential surface-modifying method that can enhance the cell affinity at the early stages in vitro.

Influence of different drying methods on microtensile bond strength of self-adhesive resin cements to dentin.

OBJECTIVE: This study investigated the effect of different drying methods of dentin surface on the bonding efficacy of self-adhesive resin cements (SRCs). MATERIALS AND METHODS: Three SRCs (RelyX U200, RU; Maxcem Elite, ME; and BisCem, BC) and one resin-modified glass ionomer cement (RelyX Luting 2, RL) were used. The characteristics of the materials were evaluated using thermogravimetric analysis and surface roughness and contact angle measurements. Human dentin surfaces were finished with 600-grit silicon carbide paper and assigned to three groups according to these drying methods: ethanol dehydration, drying by waiting for 10 s after blot-drying and blot-drying. The four cements were used for luting composite overlays to the dried dentin. After 24 h storage at 37°C and 100% relative humidity, stick-shaped specimens with a cross-sectional area of 0.8 mm(2) were prepared and stressed to failure in tension at a crosshead speed of 0.5 mm/min (n = 27). Failure modes of fractured specimens were assessed by optical and scanning electron microscopy. RESULTS: RL was the most hydrophilic, followed by BC and ME and then RU. All the luting cements luted to ethanol-dehydrated dentin showed zero bond strengths. For the three SRCs, drying by waiting produced higher microtensile bond strengths than blot-drying. RU showed the best bonding performance in the above two dentin conditions. RL showed significantly higher bond strength in blot-drying condition than in drying-by-waiting (p < 0.001). CONCLUSIONS: This study suggests that dentin surface moisture has a crucial effect on the bond strength of SRCs.

Enhanced attachment of human osteoblasts on NH3-treated poly(L-lactic acid) membranes for guided bone regeneration.

Barrier membranes for guided bone regeneration (GBR) were prepared by a solvent casting method using solutions of poly(L-lactic acid) (PLLA) and chitosan. PLLA and PLLA/chitosan membranes were treated with ammonia gas plasma. PLLA/chitosan membranes were successfully fabricated, and the surface of the PLLA/chitosan membrane was clearly modified by NH3 plasma treatment according to attenuated total reflectance (ATR-FTIR), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) analyses. Additionally, water contact angle testing indicated that the hydrophilicity of these membranes was significantly increased. MG-63 cells were cultured on each type of membrane, and cell viability was examined using an MTT assay. After one week of culturing, MG-63 cells were more abundant on PLLA/chitosan membranes than on PLLA membranes. The cell viability of PLLA/chitosan membranes with plasma treatment was significantly higher than that of PLLA membranes. These results suggest that this plasma-treated membrane is suitable for GBR and is a promising source of bioactive membrane material for bone regeneration.

Development and structure of a novel barrier membrane composed of drug-loaded poly(lactic-co-glycolic acid) particles for guided bone regeneration.

A novel barrier membrane composed of poly(lactic-co-glycolic acid) particles loaded with dexamethasone (DEX) as a bioactive molecule was produced via a modified nanoprecipitation method without any mixing. The particle membranes had a bilayer structure: one side was smooth and had a compact surface that was connected to larger particles, while the opposite side was rough, porous and connected to smaller particles. Additionally, a cross-section of the particle membrane had a porous structure with nano and micro sized irregular pores. Process optimization revealed that NaCl concentration in the water phase, with acetone as solvent and water as a non-solvent, played critical roles in determining the properties of the particle membranes, such as DEX encapsulation efficiency, thickness and surface morphologies of the particle membranes. A novel barrier membrane containing DEX using polymer particle drug capture technology has been successfully developed.

Analysis of the inorganic component of autogenous tooth bone graft material.

This study was performed to identify the calcium phosphate minerals, chemical element and Ca/P ratio and to examine the surface structure of autogenous tooth bone grafting material (AutoBT) which recently developed and applied clinically as a bone graft materials. The analytical results showed that AutoBT is composed of low-crystalline hydroxyapatite (HA) and possibly other calcium phosphate minerals, which is similar to the minerals of human bone tissues. And the dental crown portion was composed of high-crystalline calcium phosphate minerals (mainly HA) with higher Ca/P ratio while the root portion was mainly composed of low-crystalline calcium phosphates with relatively low Ca/P ratio.

Drug-loaded porous spherical hydroxyapatite granules for bone regeneration.

Porous spherical hydroxyapatite (HAp) granules, which are not only can be used for bone void filler, but also drug delivery systems, were prepared using a liquid nitrogen method. Various pore and channel structures of spherical granules were obtained by adjusting the ratio of water to HAp powder and the amount of sodium chloride (NaCl). By using the water to powder ratio at 2.0 ml/g and the amount of NaCl at 15 wt% by powder, the spherical granules have optimal pore volume, micro-channel structure and strength to handle as well as the ability to work as a drug delivery system. When the NaCl content was 15 wt%, the micro-channel structure was changed, but the pore volume was maintained. For the drug release test, dexamathasone (Dex) was loaded as a model drug on the prepared HAp granules by the immersion method, and the drug release behavior was curved by a UV/vis spectrophotometer. As a result, different drug release behavior was observed according to micro-channel structural differences. Therefore, it was concluded that the NACl could be applied as the pore and micro-channel structure control agent. Porous spherical HAp granules, which were fabricated by a liquid nitrogen method, show potential as bone void filler with the ability of controlled drug release.

Bone regeneration of tibial segmental defect using isotropic-pore structures hydroxyapatite/alumina bi-layered scaffold: in vivo pilot study.

Bone defects resulting from trauma or pathology represent a common and significant clinical problem. In this study, hydroxyapatite (HAp)-alumina bi-layered scaffolds, which have the benefits of both HAp (i.e., osteointegration, osteoconduction) and alumina (i.e., hardness) were used as a bone substitute for the repair of large segmental defects (20 mm) created in a beagle tibia model. Highly porous bi-layered scaffolds with isotropic-pore structures were fabricated using a polymer-template coating technique. The pore sizes obtained using this approach ranged between 230 µm and 470 µm, and porosity was 91.61±1.28%. Using scanning electron microscopy and energy dispersive spectroscopy, it was confirmed that the frame of each bi-layered scaffold consisted of an alumina inner layer and HAp outer layer. The evaluation of bone regeneration within each scaffold after implantation in the beagle tibia was performed using CT, micro-CT, scintigraphy. New bone formation was evident in the large segmental defects treated with HAp/alumina scaffolds. It was concluded from this study that the HAp/alumina bi-layered scaffold is instrumental in inducing host-scaffold engraftment at the distal and proximal ends of the defect as well as distributing the newly formed bone throughout each scaffold 8 weeks post-implantation.

Antibacterial Activity of Propolis-Embedded Zeolite Nanocomposites for Implant Application.

This study investigates the potential of propolis-embedded zeolite nanocomposites for dental implant application. Propolis-embedded zeolite nanocomposites were fabricated by complexation of propolis and zeolites. Then, they were pelleted with Poly(L-lactide) (PLA)/poly(ε-caprolactone) (PCL) polymer for the fabrication of a dental implant. The chemical properties of propolis were not changed during the fabrication of propolis-embedded zeolite nanocomposites in attenuated total reflection-fourier transform infra-red (ATR FT-IR) spectroscopy measurements. Propolis was continuously released from propolis-embedded zeolite nanocomposites over one month. PLA/PCL pellets containing propolis-embedded zeolite nanocomposites showed longer sustained release behavior compared to propolis-embedded zeolite nanocomposites. Propolis-embedded zeolite nanocomposite powder showed similar antibacterial activity against C. albicans in an agar plate and formed an inhibition zone as well as chlorohexidine (CHX) powder. Eluted propolis solution from PLA/PCL pellets also maintained antibacterial activity as well as CHX solution. Furthermore, eluted propolis solution from PLA/PCL pellets showed significant antibacterial efficacy against C. albicans, S. mutans and S. sobrinus. Dental implants fabricated from PLA/PCl polymer and propolis-embedded zeolite nanocomposites also have antibacterial efficacy and negligible cytotoxicity against normal cells. We suggest that PLA/PCl pellets containing propolis-embedded zeolite nanocomposites are promising candidates for dental implants.

Comparison of titanium and biodegradable miniplates for fixation of mandibular fractures.

PURPOSE: The purpose of the present study was to compare the use of biodegradable miniplates and titanium miniplates for the fixation of mandibular fractures. PATIENTS AND METHODS: BioSorb FX biodegradable plates and screws and titanium miniplates were used in 91 patients (65 males and 26 females; age range 11 to 69 years) for the treatment of mandibular fractures. The clinical and radiographic findings were recorded at 1, 3, 6, and 12 months after surgery. RESULTS: The overall complication rate was 4.41%. In the biodegradable plate group, infection occurred in 2 cases (4.26%) and was resolved by incision and drainage and antibiotics. In the titanium plate group, infection occurred in 1 case and plate fracture in 1 case (4.56%). The fractured plate was removed, and a new titanium miniplate was applied using a trocar. The infection was resolved with antibiotics. No adverse tissue reactions, malocclusions, or malunions occurred during the observation period. CONCLUSIONS: Our results have shown that the rate of morbidity is very low with the use of biodegradable plates and titanium plates, suggesting that biodegradable and titanium plates have the potential for successful use in the fixation of mandibular fractures.

Comparative study between resorbable and nonresorbable plates in orthognathic surgery.

PURPOSE: The purpose of the present study was to evaluate the clinical application of resorbable and nonresorbable plates for correction of facial asymmetry. PATIENTS AND METHODS: A total of 272 patients who had undergone orthognathic surgery were enrolled. The site of osteotomy was fixed using a nonresorbable plate in group I (n = 152) and using a resorbable plate in group II (n = 120). The postoperative complications included postoperative anterior open bite, infection, temporomandibular joint dysfunction, and postoperative relapse. The incidence of all complications was examined. RESULTS: The surgical outcome was successful in 269 patients (98.89%). Of the 152 patients with a titanium plate, 13 (8.6%) developed complications. Of the 120 patients with a resorbable plate, 22 (18.3%) developed complications. A greater degree of postoperative open bite and a trend toward relapse were observed in patients' cases in which an absorbable fixation plate was used. Postoperative infection occurred in patients with an absorbable fixation plate. CONCLUSION: On the basis of these data, we have concluded that an absorbable fixation plate should be used instead of a titanium fixation plate in indicated patients.

Influence of Curing Mode on the Surface Energy and Sorption/Solubility of Dental Self-Adhesive Resin Cements.

This study investigated the influence of curing mode (dual- or self-cure) on the surface energy and sorption/solubility of four self-adhesive resin cements (SARCs) and one conventional resin cement. The degree of conversion (DC) and surface energy parameters including degree of hydrophilicity (DH) were determined using Fourier transform infrared spectroscopy and contact angle measurements, respectively (n = 5). Sorption and solubility were assessed by mass gain or loss after storage in distilled water or lactic acid for 60 days (n = 5). A linear regression model was used to correlate between the results (%DC vs. DH and %DC/DH vs. sorption/solubility). For all materials, the dual-curing consistently produced significantly higher %DC values than the self-curing (p < 0.05). Significant negative linear regressions were established between the %DC and DH in both curing modes (p < 0.05). Overall, the SARCs showed higher sorption/solubility values, in particular when immersed in lactic acid, than the conventional resin cement. Linear regression revealed that %DC and DH were negatively and positively correlated with the sorption/solubility values, respectively. Dual-curing of SARCs seems to lower the sorption and/or solubility in comparison with self-curing by increased %DC and occasionally decreased hydrophilicity.

Bone Regeneration of Hydroxyapatite with Granular Form or Porous Scaffold in Canine Alveolar Sockets.

This study was undertaken to assess bone regeneration using hydroxyapatite (HA). The primary focus was comparison of bone regeneration between granular HA (gHA) forms and porous HA (pHA) scaffold. The extracted canine alveolar sockets were divided with three groups: control, gHA and pHA. Osteogenic effect in the gHA and pHA groups showed bone-specific surface and bone mineral density to be significantly higher than that of the control group (p<0.01). Bone volume fraction, bone mineral density, and amount of connective tissue related to disturbing osseointegration of the gHA group was higher than in the pHA group. Quantity of new bone formation of the pHA group was higher than that of the gHA group. This study demonstrated that gHA and pHA are potentially good bone substitutes for alveolar socket healing. For new bone formation during 8 weeks' post-implantation, HA with porous scaffold was superior to the granular form of HA.