ABSTRACT
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Hydroxyapatite (HA) is important in biomedical applications because of its chemical similarity to the mineral content of bone and its consequent bioactivity. Silicon substitution into the hydroxyapatite crystal lattice was found to... more
Hydroxyapatite (HA) is important in biomedical applications because of its chemical similarity to the mineral content of bone and its consequent bioactivity. Silicon substitution into the hydroxyapatite crystal lattice was found to enhance its bioactivity both in vitro and in vivo [1, 2]. However, the mechanism for the enhancement is still not well understood. In this paper, the crystal imperfections introduced by silicon substitution were studied using XRD and Raman spectroscopy. It was found that silicon substitution did not introduce microstrain, but deceased the crystal size in the hk0 direction. Three new vibration modes and peak broadening were observed in Raman spectra following silicon incorporation. The imperfections introduced by silicon substitution may play a role in enhancing bioactivity. A phenomenological relationship between the width of the PO4 v1 peak and crystal size was established.
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Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of... more
Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of particular interest was the requirement of carbon dioxide release during the setting reaction to obtain Ca(9-x)(HPO(4))(1-1.5x) (PO(4))(5-2.5x)(CO(3))(3.5x)(OH)(1 + 1.5x) with a fixed carbonate content. Results indicated that a compromise is necessary with respect to the maximum permissible level of CaCO(3) addition to the powder mixture as against appropriate setting and hardening properties. Cementlike materials with good setting and hardening properties were obtained when alpha-Ca(3)(PO(4))(2) was the main reactant using Ca(H(2)PO(4))(2) and CaCO(3) as additives in relative proportions of <10 wt % corresponding, approximately, to the stability field area (x,lambda) contained within the lines lambda = -1.5x, x = 0.3, and lambda = -1. Desirable workability and setting properties were lost as the parameters x and -lambda increased. Finally, it was also found to be virtually impossible to obtain a predetermined chemical composition for the setting apatite precipitate, since to increase the amount of carbon dioxide released from the initial powder mixture during setting, the solution pH would need to be decreased, and in doing so the nature of the precipitate could be altered to fulfil the thermodynamic conditions of the solubility diagrams of calcium phosphates.
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ABSTRACT
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ABSTRACT Four different assays, monitoring different aspects of cellular activity were used to assess the in vitro biocompatibility of three experimental zirconias (ZrO2-A, ZrO2-B and ZrO2-C) with minor chemical modifications. The assays... more
ABSTRACT Four different assays, monitoring different aspects of cellular activity were used to assess the in vitro biocompatibility of three experimental zirconias (ZrO2-A, ZrO2-B and ZrO2-C) with minor chemical modifications. The assays used were Neutral red uptake, MTT, alamarBlue and a live/dead cell stain. No cytotoxic effect was detected in the extracts from the three test zirconia samples using Neutral red uptake and MTT assays. However, a variation in response was observed in cells cultured directly on the surface of three test zirconias using the alamarBlue assay. The three test zirconia substrates showed no toxic effect after 1 and 2 days in culture. After 5 days in direct contact with the experimental zirconias, a significant decrease in cell activity was observed on sample ZrO2-B, which was confirmed by fluorescence microscopy, showing a layer of dead cells (stained by thidium homodimer-1) on the sample surface. The findings from this study indicated that great care is required when selecting assays to assess the biocompatibility of modified materials with regard to the type and sensitivity of the assay and culture conditions.
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Bioceramic specimens have been prepared by incorporating a small amount of silicon (0.4 wt %) into the structure of hydroxyapatite [Ca10(PO4)6(OH)2, HA] via an aqueous precipitation reaction to produce a silicon-substituted hydroxyapatite... more
Bioceramic specimens have been prepared by incorporating a small amount of silicon (0.4 wt %) into the structure of hydroxyapatite [Ca10(PO4)6(OH)2, HA] via an aqueous precipitation reaction to produce a silicon-substituted hydroxyapatite (Si-HA). The results of chemical analysis confirmed the proposed substitution of the silicon (or silicate) ion for the phosphorus (or phosphate) ion in hydroxyapatite. The Si-HA was produced by first preparing a silicon-substituted apatite (Si-Ap) by a precipitation process. A single-phase Si-HA was obtained by heating/calcining the as-prepared Si-Ap to temperatures above 700 degrees C; no secondary phases, such as tricalcium phosphate (TCP), tetracalcium phosphate (TeCP), or calcium oxide (CaO), were observed by X-ray diffraction analysis. Although the X-ray diffraction patterns of Si-HA and stoichiometric HA appeared to be identical, refinement of the diffraction data revealed some small structural differences between the two materials. The silicon substitution in the HA lattice resulted in a small decrease in the a axis and an increase in the c axis of the unit cell. This substitution also caused a decrease in the number of hydroxyl (OH) groups in the unit cell, which was expected from the proposed substitution mechanism. The incorporation of silicon in the HA lattice resulted in an increase in the distortion of the PO4 tetrahedra, indicated by an increase in the distortion index. Analysis of the Si-HA by Fourier transform infrared (FTIR) spectroscopy indicated that although the amount of silicon incorporated into the HA lattice was small, silicon substitution appeared to affect the FTIR spectra of HA, in particular the P-O vibrational bands. The results demonstrate that phase-pure silicon-substituted hydroxyapatite may be prepared using a simple precipitation technique.
Research Interests: Physical Chemistry, Biomedical Engineering, Hydroxyapatite, Calcium, Silicon, and 18 moreCrystallization, Structural Analysis, Biomedical, Phosphorus, Ceramics, Biomedical Materials, Chemical Analysis, Biomaterial, Precipitation, Chemical Precipitation, X ray diffraction, Fourier transform infrared spectroscopy, Substitution, Powders, Materials Testing, Durapatite, Biocompatible Materials, and *Hot Temperature(Crystallization, Structural Analysis, Biomedical, Phosphorus, Ceramics, Biomedical Materials, Chemical Analysis, Biomaterial, Precipitation, Chemical Precipitation, X ray diffraction, Fourier transform infrared spectroscopy, Substitution, Powders, Materials Testing, Durapatite, Biocompatible Materials, and *Hot Temperature)
(Crystallization, Structural Analysis, Biomedical, Phosphorus, Ceramics, Biomedical Materials, Chemical Analysis, Biomaterial, Precipitation, Chemical Precipitation, X ray diffraction, Fourier transform infrared spectroscopy, Substitution, Powders, Materials Testing, Durapatite, Biocompatible Materials, and *Hot Temperature)
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ABSTRACT
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Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of... more
Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of particular interest was the requirement of carbon dioxide release during the setting reaction to obtain Ca(9-x)(HPO(4))(1-1.5x) (PO(4))(5-2.5x)(CO(3))(3.5x)(OH)(1 + 1.5x) with a fixed carbonate content. Results indicated that a compromise is necessary with respect to the maximum permissible level of CaCO(3) addition to the powder mixture as against appropriate setting and hardening properties. Cementlike materials with good setting and hardening properties were obtained when alpha-Ca(3)(PO(4))(2) was the main reactant using Ca(H(2)PO(4))(2) and CaCO(3) as additives in relative proportions of <10 wt % corresponding, approximately, to the stability field area (x,lambda) contained within the lines lambda = -1.5x, x = 0.3, and lambda = -1. Desirable workability and setting properties were lost as the parameters x and -lambda increased. Finally, it was also found to be virtually impossible to obtain a predetermined chemical composition for the setting apatite precipitate, since to increase the amount of carbon dioxide released from the initial powder mixture during setting, the solution pH would need to be decreased, and in doing so the nature of the precipitate could be altered to fulfil the thermodynamic conditions of the solubility diagrams of calcium phosphates.
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... film deposition techniques are also being investigated including electrophoresis, solgel routes, electrochemical ... industries for many years, but its potential for bioactive coatings on ... vitro studies have shown that these... more
... film deposition techniques are also being investigated including electrophoresis, solgel routes, electrochemical ... industries for many years, but its potential for bioactive coatings on ... vitro studies have shown that these coatings exhibit enhanced bioactivity and biomineralisation ...
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Cylindrical dental implants made of commercially pure titanium were analysed in four different surface finishes: as-machined, Al2O3 blasted with Al2O3 particles, plasma-sprayed with titanium beads and electrolytically coated with... more
Cylindrical dental implants made of commercially pure titanium were analysed in four different surface finishes: as-machined, Al2O3 blasted with Al2O3 particles, plasma-sprayed with titanium beads and electrolytically coated with hydroxyapatite. Scanning electron ...
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Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of... more
Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of particular interest was the requirement of carbon dioxide release during the setting reaction to obtain Ca(9-x)(HPO(4))(1-1.5x) (PO(4))(5-2.5x)(CO(3))(3.5x)(OH)(1 + 1.5x) with a fixed carbonate content. Results indicated that a compromise is necessary with respect to the maximum permissible level of CaCO(3) addition to the powder mixture as against appropriate setting and hardening properties. Cementlike materials with good setting and hardening properties were obtained when alpha-Ca(3)(PO(4))(2) was the main reactant using Ca(H(2)PO(4))(2) and CaCO(3) as additives in relative proportions of <10 wt % corresponding, approximately, to the stability field area (x,lambda) contained within the lines lambda = -1.5x, x = 0.3, and lambda = -1. Desirable workability and setting properties were lost as the parameters x and -lambda increased. Finally, it was also found to be virtually impossible to obtain a predetermined chemical composition for the setting apatite precipitate, since to increase the amount of carbon dioxide released from the initial powder mixture during setting, the solution pH would need to be decreased, and in doing so the nature of the precipitate could be altered to fulfil the thermodynamic conditions of the solubility diagrams of calcium phosphates.
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Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of... more
Powder mixtures of alpha-Ca(3)(PO(4))(2), Ca(H(2)PO(4))(2), and CaCO(3) were investigated to assess their potential for the precipitation of a carbonated apatite suitable for cement applications from a supersaturated solution. Of particular interest was the requirement of carbon dioxide release during the setting reaction to obtain Ca(9-x)(HPO(4))(1-1.5x) (PO(4))(5-2.5x)(CO(3))(3.5x)(OH)(1 + 1.5x) with a fixed carbonate content. Results indicated that a compromise is necessary with respect to the maximum permissible level of CaCO(3) addition to the powder mixture as against appropriate setting and hardening properties. Cementlike materials with good setting and hardening properties were obtained when alpha-Ca(3)(PO(4))(2) was the main reactant using Ca(H(2)PO(4))(2) and CaCO(3) as additives in relative proportions of <10 wt % corresponding, approximately, to the stability field area (x,lambda) contained within the lines lambda = -1.5x, x = 0.3, and lambda = -1. Desirable workability and setting properties were lost as the parameters x and -lambda increased. Finally, it was also found to be virtually impossible to obtain a predetermined chemical composition for the setting apatite precipitate, since to increase the amount of carbon dioxide released from the initial powder mixture during setting, the solution pH would need to be decreased, and in doing so the nature of the precipitate could be altered to fulfil the thermodynamic conditions of the solubility diagrams of calcium phosphates.
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Research Interests: Biomaterials, Hydroxyapatite, Cell Adhesion, Titanium, Silicon, and 20 moreCrystallization, Multidisciplinary, Extracellular Matrix, Cell line, Cell morphology, In Vitro, Humans, Thin Film, Nanostructures, Actin, Particle Size, Surface Properties, Deficiency, Element, Cell Proliferation, Osteoblasts, Durapatite, Cell Survival, Cell Size, and Cell Membrane
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This chapter reviews the range of ceramics currently used in skeletal repair and tissue regeneration and covers the bioinert, bioactive and resorbable ceramics, glasses and glass ceramics. The scope of the chapter includes the... more
This chapter reviews the range of ceramics currently used in skeletal repair and tissue regeneration and covers the bioinert, bioactive and resorbable ceramics, glasses and glass ceramics. The scope of the chapter includes the relationships between microstructure (crystalline and non-crystalline) and properties (mechanical properties, surface properties, biocompatibility and bioactivity). The processing (porous tissue engineering scaffolds and surface modification) of bioceramics is also considered. Based on the stringent requirements for clinical application, prospects for the development of advanced ceramic materials for tissue engineering are highlighted for the future.
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The potential applications of ice-templating porous materials are constantly expanding, especially as scaffolds for tissue engineering. Ice-templating, a process utilizing ice nucleation and growth within an aqueous solution, consists of... more
The potential applications of ice-templating porous materials are constantly expanding, especially as scaffolds for tissue engineering. Ice-templating, a process utilizing ice nucleation and growth within an aqueous solution, consists of a cooling stage (before ice nucleation) and a freezing stage (during ice formation). While heat release during cooling can change scaffold isotropy, the freezing stage, where ice crystals grow and anneal, determines the final size of scaffold features. To investigate the path of heat flow within collagen slurries during solidification, a series of ice-templating molds were designed with varying the contact area with the heat sink, in the form of the freeze drier shelf. Contact with the heat sink was found to be critical in determining the efficiency of the release of latent heat within the perspex molds. Isotropic collagen scaffolds were produced with pores which ranged from 90 μm up to 180 μm as the contact area decreased. In addition, low-temperature ice annealing was observed within the structures. After 20 h at -30 °C, conditions which mimic storage prior to lyophilization, scaffold architecture was observed to coarsen significantly. In future, ice-templating molds should consider not only heat conduction during the cooling phase of solidification, but the effects of heat flow during ice growth and annealing.
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An investigation was performed with the objective of determining the effects of adding calcium-phosphate based materials of varying Ca:P ratios on the sintering characteristics and phase composition of hydroxyapatite. Samples were... more
An investigation was performed with the objective of determining the effects of adding calcium-phosphate based materials of varying Ca:P ratios on the sintering characteristics and phase composition of hydroxyapatite. Samples were prepared from a commercially available hydroxyapatite (Plasma Biotal, U.K.) and two Ca-P additives, CAP1 and CAP2. Compacts were then pressed and sintered at 1300°C for 2 hours and characterised by measurements of linear shrinkage, density, and X-ray diffraction. The results were compared with those for pressed and sintered hydroxyapatite, which served as a control. The CAP2-HA underwent a greater degree of shrinkage and densification than both CAP1-HA and as-received HA, demonstrating its potential as a sintering aid. Furthermore, X-ray diffraction patterns demonstrated that there was minimal decomposition of the HA to TCP in the CAP2-HA than in the CAP1-HA, and preliminary strength tests indicated that the CAP2 additions reinforced the HA.
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Bioceramics 15: Ultrastructural Characterisation of Hydroxyapatite and Silicon-Substituted Hydroxyapatite.
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Abstract. The production of nano-scale hydroxyapatite (HA) suspensions to be used for the reticulated foam method of scaffold production was investigated at temperatures of between 10 and 60 O C. An increase in reaction temperature was... more
Abstract. The production of nano-scale hydroxyapatite (HA) suspensions to be used for the reticulated foam method of scaffold production was investigated at temperatures of between 10 and 60 O C. An increase in reaction temperature was associated with an increase in the particle ...
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Calcium phosphate cements have been the subject of many studies in the last decade because of their biocompatibility, their capacity to fill bone cavities and their hardening properties; properties which are desirable in a broad range of... more
Calcium phosphate cements have been the subject of many studies in the last decade because of their biocompatibility, their capacity to fill bone cavities and their hardening properties; properties which are desirable in a broad range of surgical applications. The setting and hardening of these materials are controlled by dissolution-precipitation chemical reactions at room or body temperature and involve crystalline phase transformations.
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The initial setting properties of calcium phosphate cements in the CaHPO4-alpha-Ca3(PO4)2 (DCP-alpha-TCP) system have been investigated. Interest was focused on the pH, workability, cohesion time and initial and final setting times. The... more
The initial setting properties of calcium phosphate cements in the CaHPO4-alpha-Ca3(PO4)2 (DCP-alpha-TCP) system have been investigated. Interest was focused on the pH, workability, cohesion time and initial and final setting times. The addition of CaCO3 modified the structure of the cement reaction product such that it became more similar to the apatite phase in bone mineral. The addition of 10% w/w of CaCO3 reduced the viscosity of the cement pastes resulting in an increase in initial and final setting times and improved injectability.
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The effect of different calcination temperatures on the powder characteristics and the sintered density of synthetic hydroxyapatite (HA) powders, produced using two different processing routes, was examined. Powders were produced by... more
The effect of different calcination temperatures on the powder characteristics and the sintered density of synthetic hydroxyapatite (HA) powders, produced using two different processing routes, was examined. Powders were produced by either drying, milling and sieving an as-precipitated HA or by spray-drying a slurry of precipitated HA. Calcining the two powders at temperatures between 400 and 1000 degrees C did not significantly affect the powder particle size. The specific surface areas of the two powders, however, were reduced from 70-80 m2/g for a calcination temperature of 400 degrees C to approximately 5-7 m2/g for 1000 degrees C. Analysis of the surfaces of the HA powders using scanning electron microscopy (SEM) illustrated the coarsening and subsequent sintering of the sub-micron crystallites that constitute a powder particle as the calcination temperature increased, corresponding to the decrease in surface area of the powders. The sintered densities of the final ceramics wer...
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Titanium-zirconium based alloys containing a small amount of niobium were investigated in order to evaluate their possible use as biomedical materials. Zirconium, which belongs to the IVa group, is known to have good corrosion resistance... more
Titanium-zirconium based alloys containing a small amount of niobium were investigated in order to evaluate their possible use as biomedical materials. Zirconium, which belongs to the IVa group, is known to have good corrosion resistance and biocompatibility similar to titanium. As the titanium-zirconium system shows a complete solid solution, a wide variation of alloy design is available and large quantities of solid-solution hardening must be possible. Niobium, having a beta-phase stabilizing effect, was chosen as a ternary element in order to control desirably the microstructure. There have been no reports which suggest its harm to a living body. The alloys containing 2% or 3% niobium showed the highest hardness value after aging heat treatment at 773 K. In contrast to this, no alteration of hardness was seen in specimens aged at 1073 K. Through conventional X-ray diffractometry and in situ X-ray analysis using a hot stage, beta-phase precipitation in the A matrix was identified....
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The structural changes that occur during the transformation of a Ca-deficient apatite, prepared by a wet chemical method, to beta-TCp were investigated. X-ray diffraction (XRD) analysis of as-prepared samples and samples calcined at... more
The structural changes that occur during the transformation of a Ca-deficient apatite, prepared by a wet chemical method, to beta-TCp were investigated. X-ray diffraction (XRD) analysis of as-prepared samples and samples calcined at temperatures between 500 and 1100 degrees C showed that the transformation occurs over the temperature range 710-740 degrees C, under non-equilibrium conditions. The change in crystallite size with increasing calcination/sintering temperature was studied by XRD using the Scherrer formula. Fourier transform infra-red (FTIR) analysis indicated considerable structural change in samples above and below this temperature range. Changes were observed in the hydroxyl, carbonate and phosphate bands as the calcination temperature was increased from 500 to 1100 degrees C. Even once a single beta-TCP phase is obtained at 740 degrees C there remains a considerable amount of structural change at temperatures between 740 and 1100 degrees C. This effect was illustrated ...
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Research Interests: Granules()
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Hydroxyapatite has been considered for use in the repair of osseous defects for the last 20 years. Recent developments have led to interest in the potential of porous hydroxyapatite as a synthetic bone graft. However, despite considerable... more
Hydroxyapatite has been considered for use in the repair of osseous defects for the last 20 years. Recent developments have led to interest in the potential of porous hydroxyapatite as a synthetic bone graft. However, despite considerable activity in this field, regarding assessment of the biological response to such materials, the basic materials characterization is often inadequate. This paper documents the characterization of the chemical composition, mechanical integrity, macro- and microstructure of a porous hydroxyapatite, Endobon (E. Merck GmbH), intended for the bone-graft market. Specimens possesed a range of apparent densities from 0.35 to 1.44 g cm(-3). Chemical analysis demonstrated that the natural apatite precursor of Endobon was not converted to pure hydroxyapatite, but retained many of the ionic substituents found in bone mineral, notably carbonate, sodium and magnesium ions. Investigation of the microstructure illustrated that the struts of the material were not ful...
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Phase pure hydroxyapatite (HA) and a 0.8 wt % silicon substituted hydroxyapatite (SiHA) were prepared by aqueous precipitation methods. Both HA and SiHA were processed into granules 0.5-1.0 mm in diameter and sintered at 1200 degrees C... more
Phase pure hydroxyapatite (HA) and a 0.8 wt % silicon substituted hydroxyapatite (SiHA) were prepared by aqueous precipitation methods. Both HA and SiHA were processed into granules 0.5-1.0 mm in diameter and sintered at 1200 degrees C for 2 h. The sintered granules underwent full structural characterization, prior to implantation into the femoral condyle of New Zealand White rabbits for a period of 23 days. The results show that both the HA and SiHA granules were well accepted by the host tissue, with no presence of any inflammatory cells. New bone formation was observed directly on the surfaces and in the spaces between both HA and SiHA granular implants. The quantitative histomorphometry results indicate that the percentage of bone ingrowth for SiHA (37.5%+/-5.9) was significantly greater than that for phase pure HA (22.0%+/-6.5), in addition the percentage of bone/implant coverage was significantly greater for SiHA (59.8%+/-7.3) compared to HA (47.1%+/-3.6). These findings indic...
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We describe the production of collagen fibre bundles through a multi-strand, semi-continuous extrusion process. Cross-linking using an EDC (1-ethyl-3-(3-dimethylaminopropyl)carbodiimide), NHS (N-hydroxysuccinimide) combination was... more
We describe the production of collagen fibre bundles through a multi-strand, semi-continuous extrusion process. Cross-linking using an EDC (1-ethyl-3-(3-dimethylaminopropyl)carbodiimide), NHS (N-hydroxysuccinimide) combination was considered. Atomic Force Microscopy (AFM) and Raman spectroscopy focused on how cross-linking affected the collagen fibrillar structure. In the cross-linked fibres, a clear fibrillar structure comparable to native collagen was observed which was not observed in the non-cross-linked fibre. The amide III doublet in the Raman spectra provided additional evidence of alignment in the cross-linked fibres. Raman spectroscopy also indicated no residual polyethylene glycol (from the fibre forming buffer) or water in any of the fibres.
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Levator palpebrae superioris (LPS) is a muscle responsible for lifting the upper eyelid and its malfunction leads to a condition called "ptosis", resulting in disfigurement and visual impairment. Severe ptosis is generally... more
Levator palpebrae superioris (LPS) is a muscle responsible for lifting the upper eyelid and its malfunction leads to a condition called "ptosis", resulting in disfigurement and visual impairment. Severe ptosis is generally treated with "brow-suspension" surgery, whereby the eyelid is cross-connected to the mobile tissues above the eyebrow using a cord-like material, either natural (e.g. fascia lata harvested from the patient) or a synthetic cord. Synthetic brow-suspension materials are widely used, due to not requiring the harvesting of fascia lata that can be associated with pain and donor-site complications. The mechanical properties of some commonly-used synthetic brow-suspension materials were investigated--namely, monofilament polypropylene (Prolene®), sheathed braided polyamide (Supramid Extra® II), silicone frontalis suspension rod (Visitec® Seiff frontalis suspension set), woven polyester (Mersilene® mesh), and expanded polytetrafluoroethylene (Ptose-Up)....