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Influence of polymerization initiator for base monomer on microwave curing of composite resin inlays.

Microwave polymerization was used to make composite resin inlays and the effect examined of the concentration of polymerization initiator for the base monomer. The monomers used were 2,2-bis [4-(3-methacriloxy-2-hydroxypropoxy) phenyl] propane (Bis-GMA) and triethyleneglycol dimethacrylate (TEGDMA). Bis-GMA and TEGDMA were mixed in a ratio of 6:4 by weight and were separated into five groups. To each group was added benzoyl peroxide (BPO) in the ratios of 0.1, 0.3, 0.5, 0.7 and 0.9 wt% as the polymerization initiator. These were used as the base monomers. The results showed that the degree of conversion of the cured sample increased with increasing concentration of BPO from 0.1 to 0.5 wt%, however there was no significant difference at 0.5, 0.7 and 0.9 wt% (P> 0.01). Compression strength, diametral tensile strength and the Knoop hardness showed a similar tendency as the degree of conversion. No significant difference was recorded in the Knoop hardness between the top and the bottom surfaces (P> 0.01), which suggested a uniform polymerization in the cured sample. Thus, microwave polymerization would be an efficacious method for making resin inlays with the addition of BPO to the base monomer (Bis-GMA:TEGDMA, 6:4). The maximum conversion was found at a concentration of 0.5 wt%.

Benzoyl Peroxide↗

Mechanical characterisation of three percutaneous vertebroplasty biomaterials.

Percutanous vertebroplasty (PVP) is gaining popularity for the treatment of vertebral compression fractures. The need of obtaining low viscosity materials for injection through small bore needles and the necessity of visualising the fluid flow during injection have led users to the formulation of a number of ad-hoc recipes aimed at adapting PMMA cements for this use. Industry, on its part, has addressed these requirements by developing specific products for this application. This study aimed at providing a direct comparison of a wide range of mechanical properties between three commercially available biomaterials developed for PVP: two PMMA based materials, Osteopal V (Merck Biomaterial GMBH, Dermstedt, D) and Verterbroplastic (DePuy Acromed, Inc, MA, USA), and a Bis-GMA composite, Cortoss (Orthovita, PA, USA). Cortoss consistently exhibited higher values for compressive strength, bending modulus and shear strength to both Osteopal V and Vertebroplastic. The creep behaviour of Cortoss was also different from that of the two PMMA cements.PVP can take advantage from the development of new injectable biomaterials in response to the problems associated with the use of PMMA in a highly vascularised area such as the vertebral body. In addition careful modulation of the mechanical properties of the material has the potential to further improve the outcome of PVP, possibly reducing the risk of adjacent level fractures associated with the procedure.

Biocompatible Materials↗

High-humidity performance of paperboard after treatment with xylanase, endoglucanse, and their combination.

For paperboard used to produce packaging, treatment of its fiber constituents with commercial enzymes can improve its compressive strength under cycling and high-humidity conditions. Xylanase that selectively removes pulp xylan (ca. 2% of the pulp by mass) yielded most of the observed beneficial effects, which did not appear related to the packing of the fiber network in the sheet or to the uptake of moisture at high humidity. There was also a marginal increase in the drainability of the pulp slurry, which may increase the rate of papermaking. Although endoglucanase activity also enhances certain pulp properties, there was little benefit in adding it to the xylanase treatment.

Cellulase↗

Graft copolymers of methyl methacrylate and poly([R]-3-hydroxybutyrate) macromonomers as candidates for inclusion in acrylic bone cement formulations: Compression testing.

Graft copolymers of methyl methacrylate and biodegradable, biocompatible bacterial poly([R]-3-hydroxybutyrate) (PHB) blocks were synthesized and evaluated as possible constituents in acrylic bone cements for use in orthopaedic applications. The copolymers were produced by conventional free radical copolymerization and incorporated in one commercially available acrylic bone cement brand, Antibiotic Simplex (AKZ). Cements with formulations containing 6.7 and 13.5 wt % of PMMA-graft-PHB were prepared. The morphology of the graft copolymer particles was suggested to influence the ability of the modified cement to be processed. Formulations containing more than about 20 wt % of the graft copolymer resulted in cement doughs that, both after first preparation and several hours later, were either sandy or soft spongy in texture and, thus, would be unacceptable for use in orthopaedic applications. The morphologies of the powders and the volumetric porosity (p) and ultimate compressive strength (UCS) of the cured cements were determined. Micro computed tomography showed that the cements presented average porosities of 13.5-16.9%. It was found that, while the powder particle shape and size for the experimental cements were markedly different from those of AKZ, there was no significant difference in either p or UCS for these cements. The latter was determined to be about 85 MPa for the modified cements and 84 MPa for Antibiotic Simplex. Furthermore, the UCS of all the cements exceeded the minimum level for acrylic bone cements, as stipulated by ASTM F-451.

Biocompatible Materials↗

Incadronate inhibits osteoporosis in ovariectomized rats.

Incadronate is a highly effective inhibitor of stimulated bone resorption as demonstrated in a hypercalcemia model in rats, bone metastasis models in mice and rats, and an osteoporosis model in dogs. In this study, the effect of incadronate on osteoporosis in ovariectomized rats was examined. Incadronate dose-dependently inhibited decreases in second lumbar vertebrae bone mineral density (BMD) following oral administration for 4 or 12 weeks. Significant inhibition was observed at doses of more than 0.3 mg/kg. Incadronate dose-dependently inhibited the loss of distal femur metaphyseal compressive strength following 12 weeks of oral administration, and this was significant at a 3 mg/kg daily dose. Incadronate also dose-dependently inhibited the increases in urinary deoxypyridinoline levels after 4-or 12-week oral administrations. While incadronate had no effect on serum osteocalcin levels after 4 weeks of oral administration, it did dose-dependently reduce levels after 12 weeks of oral administration. These results suggested that incadronate may be a useful drug for osteoporosis due to stimulated bone resorption.

Administration, Oral↗

Characterization of a novel calcium phosphate/sulphate bone cement.

Apatitic cements have shown excellent biocompatibility and adequate mechanical properties but have slow resorption in the human body. To assure that new bone tissue grows into the bone defect, a certain porosity is necessary although hard to achieve in injectable cements with suitable mechanical properties. An attempt was made by mixing alpha-tricalcium phosphate (alpha-TCP), calcium sulphate hemihydrate (CSH) and an aqueous solution containing 2.5 wt% of Na(2)HPO(4). The aim was to obtain a material containing two phases: a) one apatitic phase (calcium-deficient hydroxyapatite; CDHA) and b) one resorbable phase (calcium sulphate dihydrate; CSD). alpha-TCP and CSH mixtures were produced at relative intervals of 20 wt%. The liquid-to-powder (L/P) ratio to obtain a paste was 0.32 mLg(-1). The highest compressive strength (34 MPa) was obtained for the pure alpha-TCP sample. The strength was, in a first approximation, directly correlated to the weight proportions of the powders. X-ray diffraction analysis showed that the relative intensity for CDHA increased linearly, and the one for CSD decreased exponentially, when the amount of alpha-TCP increased. Thus, CSH ceased to transform to CSD when the amount of alpha-TCP increased. Observations in environmental scanning electron microscopy confirmed the X-ray diffraction results. CSH-crystals (100 microm) were embedded in the HA-matrix permitting gradual porosity in the material when resorbed.

Biocompatible Materials↗

Bioactive PMMA bone cement prepared by modification with methacryloxypropyltrimethoxysilane and calcium chloride.

Bone cement consisting of polymethylmethacrylate (PMMA) powder and methylmethacrylate (MMA) liquid is used extensively for fixation of implants such as artificial hip joints with living bone. This type of cement, however, does not show direct bonding to the living body, and hence the fixation is liable to loosen over a long implantation period. Bioactive materials have received much attention because of their capability for bone-bonding, i.e., bioactivity, when implanted in bony defects. Osteoconduction of the bioactive materials is caused by formation of a bone-like apatite layer through a surface reaction between the material and surrounding body fluid. The apatite formation can be induced by a silanol (Sibond;OH) group formed on the materials as well as a dissolution of calcium ion (Ca(2+)) from the material. Incorporation of alkoxysilane and calcium chloride (CaCl(2)) may provide PMMA bone cement with bioactivity, because alkoxysilane gives Sibond;OH after hydrolysis, whereas CaCl(2) releases Ca(2+). In this study, we investigated the potential on bioactivity of the modified PMMA bone cement with alkoxysilane and calcium chloride. PMMA powder was mixed with various amounts of CaCl(2), and MMA liquid with various amounts of 3-methacryloxypropyltrimethoxysilane (MPS). The mixed paste was immersed in a simulated body fluid (Kokubo solution) that has a similar concentration in inorganic constituents to human blood plasma. After soaking for various periods, apatite formation on the cement was examined. Apatite formation was observed by the addition of CaCl(2) with contents of 16 mass % and more. Incorporation of MPS accelerates the apatite formation. Setting time of the cement was significantly elongated after the addition of MPS, whereas compressive strength significantly decreased with increasing the contents of CaCl(2) and MPS. The hardened cement containing 20 mass % of CaCl(2) in the powder and 20 mass % of MPS in the liquid showed a tendency to be more osteoconductive to living bone after implantation in rabbit tibiae than the unmodified cement. These results indicate that bioactivity of the modified PMMA bone cement increases with increasing amounts of MPS and CaCl(2). Bioactive bone cement is successfully obtained when it contains appropriate concentrations of alkoxysilane and calcium chloride.

Animals↗

Effects of long-term storage on properties of an alginate impression material.

STATEMENT OF PROBLEM: Storage stability is a critical characteristic for perishable dental materials. PURPOSE: The purpose of this shelf-life study was to document changes in the properties of an alginate impression material on exposure to various environmental conditions for more than 78 months. MATERIAL AND METHODS: Properties measured included recovery from deformation, strain in compression, compressive strength, tear strength, working time, and creep compliance. RESULTS: Results revealed increases in strength and working time and a decrease in recovery from deformation at 30 to 50 months: strength and recovery then remained constant past 6 years, whereas working time and creep compliance decreased. Only the most stressful environmental conditions (heat and humidity) caused spontaneous failure of the material to set. CONCLUSIONS: We concluded that, under most storage conditions, properties of the alginate material tested remain within ADA specification limits well past manufacturer's designated shelf life. ADA specifications should require manufacturers to verify that the shelf life of each perishable material is based on valid data. An accelerated aging test was developed to simulate real time property changes and to assist in evaluating similar materials.

Alginates↗

An inexpensive alternative approach to bone compression analyses.

A new method for testing the compression strength of vertebrae was developed and implemented using minimal resources and time expenditure. The device digitally measured and analyzed the torque and force necessary to load rat lumbar and thoracic vertebrae to failure. The system was calibrated using a series of known lead masses. Similar to other standardized force/compression and torque devices, this method has been shown to provide reliable and reproducible results. Furthermore, although vertebrae were the only specimens used to collect data in these initial studies, this measurement system could be altered quite easily to allow for a variety of test materials.

Animals↗

Three-dimensional aqueous-derived biomaterial scaffolds from silk fibroin.

A new all-aqueous process is described to form three-dimensional porous silk fibroin matrices with control of structural and morphological features. The result of this process are scaffolds with controllable porosity and pore sizes that fully degrade in the presence of proteases, unlike prior methods to generate silk-based biomaterials that required the use of organic solvent treatments to impart control of structure and stability in aqueous environments, with low rates of proteolytic hydrolysis. A mechanism is proposed for this novel process that imparts physical stability via hydrophobic interactions. Adjusting the concentration of silk fibroin in water, and the particle size of granular NaCl used in the process, leads to the control of morphological and functional properties of the scaffolds. The aqueous-derived scaffolds had highly homogeneous and interconnected pores with pore sizes ranging from 470 to 940 microm, depending on the mode of preparation. The scaffolds had porosities >90% and compressive strength and modulus up to 320 +/- 10 and 3330 +/- 500 KPa, respectively, when formed from 10% aqueous solutions of fibroin. The scaffolds fully degraded upon exposure to protease during 21 days, unlike the scaffolds prepared from organic solvent processing. These new silk-based three-dimensional matrices provide useful properties as biomaterial matrices due to the all-aqueous mode of preparation, control of pore size, connectivity of pores, degradability and useful mechanical features. Importantly, this process offers an entirely new window of materials properties when compared with traditional silk fibroin-based materials.

Absorbable Implants↗

Gelatin blends with alginate: gels for lipase immobilization and purification.

Blends of natural polysaccharide sodium alginate (5%) with gelatin (3%) cross-linked with glutaraldehyde provide beads with excellent compressive strength (8 x 10(4) Pa) and regular structure on treatment with calcium chloride. Lipases from porcine pancreas, Pseudomonas cepacia, and Candida rugosa were immobilized in such a blend with excellent efficiency. The immobilized enzymes were stable and were reused several times without significant loss of enzyme activity both in aqueous and reverse micellar media. The beads were functionalized with succinic anhydride to obtain beads with extra carboxylic acid groups. These functionalized beads were then successfully used for 7.4-fold purification of crude porcine pancreatic lipase in a simple operation of protein binding at pH 5 and release at pH 8.5.

Alginates↗

Factors influencing calcium phosphate cement shelf-life.

Long-term stability during storage (shelf-life) is one major criterion for the use of a material as medical device. This study aimed to investigate the ageing process of beta-tricalcium phosphate/monocalcium phosphate cement powders when stored in sealed containers at ambient conditions. This kind of cement type is of interest because it is forming dicalcium phosphate dihydrate (brushite) when set, which is in contrast to hydroxyapatite resorbable in physiological conditions. The stability of cements was checked by either measuring the phase composition of powders as well as the setting time and compressive strength when mixed with sodium citrate as liquid. Critical factors influencing ageing were found to be temperature, humidity and the mixing regime of the powders. Mechanically mixed cement powders which were stored in normal laboratory atmosphere (22 degrees C, 60% rel. humidity) converted to dicalcium phosphate anhydrous (monetite) within a few days; this could be mechanistically related to a dissolution/precipitation process since humidity condensed on the particles' surfaces and acted as reaction medium. Various storage conditions were found to be effective in prolonging cement stability which were in order of effectiveness: adding solid citric acid retardant>dry argon atmosphere=gentle mixing (minimal mechanical energy input) low temperature.

Biocompatible Materials↗

Calcium phosphate cement reinforced by polypeptide copolymers.

Water-based calcium phosphate with bone repairing capability was reinforced by polypeptide graft copolymers and micelles that were formed by polypeptide copolymers. The mechanical studies showed that the compression strength and fracture energy of the calcium phosphate cement (CPC)/polypeptide composites are appreciably higher than those of CPC. The molecular structure of the polypeptide graft copolymers and the association form of the polypeptide copolymers exhibit a marked effect on the mechanical properties of CPC/polypeptide composites. The polypeptide copolymers with more hydrophilic side chains and with core-shell micelle forms have more effective reinforcement effect. The morphological studies based on the scanning electron microscope (SEM) observations revealed that both polypeptide graft copolymers and polypeptide copolymer micelles are well dispersed in CPC matrix. According to the obtained experimental results, reinforcement mechanism was suggested.

Biocompatible Materials↗

Mechanical properties and in vitro biocompatibility of porous zein scaffolds.

A porous scaffold utilizing hydrophobic protein zein was prepared by the salt-leaching method for tissue engineering. The scaffolds possessed a total porosity of 75.3-79.0%, compressive Young's modulus of (28.2+/-6.7)MPa-(86.6+/-19.9)MPa and compressive strength of (2.5+/-1.2)MPa-(11.8+/-1.7)MPa, the percentage degradation of 36% using collagenase and 89% using pepsin during 14 days incubation in vitro. The morphology of pores located on the surface and within the porous scaffolds showed good pore interconnectivity by scanning electron microscopy (SEM). Rat mesebchymal stem cells (MSCs) could adhere, grow, proliferate and differentiate toward osteoblasts on porous zein scaffold. With the action of dexamethasone, the cells showed a relative higher activity of alkaline phosphatase (ALP) and a higher proliferating activity (p<0.05) than those of MSCs without dexamethasone.

Alkaline Phosphatase↗

Novel injectable calcium phosphate/chitosan composites for bone substitute materials.

In this study, a novel injectable bone substitute material was developed which consists of chitosan, citric acid and glucose solution as the liquid phase, and tricalcium phosphate powder as the solid phase. This material was moldable because of its paste consistency after mixing. We used four groups of cement to investigate the mechanical properties and biocompatibility of the new biomaterial in vitro, which were named group A (10% citric acid), B (15% citric acid), C (20% citric acid) and D (25% citric acid). The setting times of the cements were 5-30 min. X-ray diffraction analysis showed that the products were hydroxyapatite (HA) and dicalcium phosphate anhydrous. When the concentration of citric acid was increased, the compressive strength of specimen increased. Through the simulated body fluid test, we observed the material was bioactive. Group D could induce Ca and P ions to deposit the surface group D quickly. These results indicated that the concentration of citric acid in the liquid component affected the mechanical properties and bioactivity of cements. The cell cultivation test showed that the cytocompatibility of the new biomaterial was good. The method for preparing the novel bone substitute material is simple. The starting material is more readily available and cheaper than HA, poly(methyl methacrylate), and so on. The cement could have good prospects for medical application.

Animals↗

Material characterization and in vivo behavior of silicon substituted alpha-tricalcium phosphate cement.

The possibility and biological effects of substituting silicon in alpha-tricalcium phosphate (alpha-TCP) by way of solid-state reaction have been evaluated. alpha-TCP powders with varying substitution amounts (1 and 5 mol % Ca2SiO4) were synthesized by reacting mixtures of CaCO3, Ca2P2O7, and SiO2, at a rate of 4 degrees C(min)(-1) to 1100 degrees C, left to dwell for 2 h and then heated to 1325 degrees C at 4 degrees C(min)(-1) and left to dwell for a period of 4 h. The powders were then rapidly quenched in air. Si incorporation could be verified by X-ray diffraction analysis, indicating an increase of the lattice volume with increasing Si content from 4284.1(8) to 4334(1) A3 for pure alpha-TCP and alpha-Si5%TCP, respectively. The hydrolysis of milled alpha-SiTCP powders was monitored by isothermal calorimetry, and the compressive strength of set cements was tested. The results showed changes in speed and amount of heat released during reactivity tests and a decrease in mechanical strength (60, 50, and 5 MPa) with increasing Si content. In vitro bioactivity of the set cements after soaking in simulated body fluid for 4 weeks was also tested. The formation of a bonelike apatite layer on the surface of the set cements could be observed and was thickest for 1%Si (20 microm). These results were in good agreement with the in vivo studies performed, which showed strong evidence that the cement containing 1% silicon doped alpha-TCP enhanced mesenchymal cell differentiation and increased osteoblast activity compared with alpha-TCP.

Animals↗

Detrimental effect of aging on the endurance of bone cement. An in vivo and in vitro study in rabbits.

We investigated the effect of aging on the compressive strength of bone cement under in vivo and in vitro conditions. Cement molds were implanted in the dorsum of rabbits and other molds were kept under stable conditions and in darkness. Comparative measures taken at 15 days and 1, 3, 6, 12 and 24 months showed lower endurance of the implanted molds (p < 0.001). A reactive capsule surrounded the bone cement in vivo up to the 3rd month, its cellularity increased, and then almost disappeared by 1 year. Macrophages and foreign body cells reappeared at 2 years, indicating a "chemical aging" effect in the in vivo environment. Our findings suggest that aging may play an important role in the amelioration of the mechanical properties of bone cement.

Animals↗

Development of hydroxyapatite bone scaffold for controlled drug release via poly(epsilon-caprolactone) and hydroxyapatite hybrid coatings.

A scaffold-coating design, the hydroxyapatite (HA) porous bone scaffold coated with poly(epsilon-)caprolactone (PCL) and HA powder hybrids, was developed for use as tissue-regeneration and controlled-release system. An antibiotic drug, tetracycline hydrochloride (TCH), was encapsulated within the hybrid coating layer through a dip-coating and solvent-casting method. Coating cycle and drug loading amount differed to control the level of drug-release rate. The HA scaffold framework, obtained by a polymeric foam reticulate method, exhibited a highly porous structure, with porosity and pore size of approximately 87% and 180 microm, respectively. The hybrid layer, consisting of PCL sheet and HA fine powders, was uniformly coated on the scaffold surface. The coating layer exhibited only PCL and HA phases and structures, revealing no chemical interaction among the coating components, as observed by X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) analyses. The coated-HA scaffolds showed an effective stress distribution behavior in response to an applied load, as confirmed by the compressive stress-strain curve. The mechanical properties of the coated scaffolds were improved highly with coatings; the compressive strength and elastic modulus of the cyclic coated scaffolds were approximately 3-4 times, and the energy absorption were approximately 8 times, higher than those without coating. These improvements were attributed mainly to the shielding of framework flaws by a flexible coating layer and partially to the thicker stems (porosity reduction). The dissolution of the coated scaffolds in a phosphate-buffered saline (PBS) solution increased with incubation time. The drug was released sharply within the initial several hours ( approximately 2 h), but the rate decreased further, showing a sustained release. The release amount was well controlled via coating-cycle and initial drug loading amount, suggesting the effectiveness of the coating-scaffold design as a drug-delivery system.

Bone and Bones↗