Biomedical subjects

J C Knowles

Publications and source records attributed to J C Knowles.

At least 55 records · Page 3Linked to original sources

PubMed2000

Structural insights of glass-reinforced hydroxyapatite composites by Rietveld refinement.

Phase transformations and interstitial and/or substitution of trace elements during the liquid-phase sintering process of P2O5-CaO-MgO glass-reinforced hydroxyapatite (GR-HA) composites were examined by X-ray diffraction and Rietveld analyses. Using the Rietveld method for structure refinement, changes in the lattice parameters of the two main phases of the composites, hydroxyapatite (HA) and beta-tricalcium phosphate (beta-TCP), as well as changes in several bond lengths and in the occupancy of the hydroxyl oxygen site in the HA phase structure were assessed. The glasses gave rise to formation of between approximately 45 and 50% of beta-TCP, with evidence for the Mg2+ enhancing the formation of beta-TCP. Between 1,300 and 1,350 degrees C, the beta-TCP inverts to alpha-TCP, without further decomposition of the residual HA. The glasses showed evidence for stabilisation of the hydroxyl group located in the hydroxyl channels. This is supported by measurements of the hydroxyl channel radius (Rc), the Ca2-OH bond length and the hydroxyl oxygen occupancy (Oocc). Results showed that the Mg2+ containing glasses induced the beta-TCP phase formation in the structure of GR-HA composites and retarded the beta-TCP into alpha-TCP transformation at higher temperatures. The chemical composition of the P2O5 glasses also induces modifications in the lattice parameters of the crystallographic phases present in the microstructure of the composites. This suggests some substitution of Mg2 + -for-Ca2+ in the beta-TCP structure during the liquid-phase sintering process.

Biocompatible Materials↗

PubMed2000

Flow cytometry analysis of the effects of pre-immersion on the biocompatibility of glass-reinforced hydroxyapatite plasma-sprayed coatings.

Multilayered coatings composed of mixtures of HA and P2O5-based bioactive glasses are of potential clinical benefit in orthopaedic and dental surgery. Pre-immersion of these materials has been reported to further enhance their efficacy in vivo, although the precise biological effects of this treatment are not yet known. In this study we have therefore prepared double-layer plasma-sprayed coatings and evaluated the effects of pre-immersion on the growth and function of human osteosarcoma cells in vitro, using the MTT assay and flow cytometry analysis, respectively. The results showed that the increase in numbers of viable cells was the same or elevated following incubation on the pre-immersed HA and glass-reinforced HA coatings compared with the non-immersed materials. In addition, the expression of bone sialoprotein and fibronectin, two key connective tissue antigens, was up-regulated in cultures grown on the pre-immersed surfaces compared with the non-treated materials. Moreover, cell numbers and antigen expression both improved as the proportion of glass increased, particularly in the pre-immersed samples. Our findings thus suggest that the immersion treatment of these materials appeared to improve the response of these bone-like cells.

Biocompatible Materials↗

PubMed2000

Development of soluble glasses for biomedical use Part II: the biological response of human osteoblast cell lines to phosphate-based soluble glasses.

Soluble glasses are considered to be of potential clinical value in orthopaedic and dental surgery. However, the biological response to these materials is not well understood. To determine the effects of these glasses, two human osteoblast cell lines, MG63 and HOS (TE85), were incubated in vitro in the presence of increasing concentrations of extracts of the glasses. The effects of the extracts on cell growth was measured using the MTT assay and an ELISA assay was used to measure the expression of bone sialoprotein (BSP), osteonectin (ON) and fibronectin (FN), antigens which play a fundamental part in the integrity and function of hard connective tissue. The results showed that the proliferation of the cells was adversely affected only by the more soluble glasses, which also down-regulated the expression of the bone-associated proteins. In contrast, the extract of the glass with the lowest dissolution rate, which contains relatively elevated levels of Ca2+, was found to enhance bone cell growth and antigen expression. These findings suggest that the compositions of these glasses at least partly determine the response of cells and thus, that the glasses could be modified to elicit a more optimal biological response and clinical efficacy.

Journal Article↗

PubMed2000

Development of soluble glasses for biomedical use Part I: in vitro solubility measurement.

In this study soluble glasses have been developed for biomedical applications containing P2O5 as a network former and CaO and Na2O as modifiers. This study shows that as expected, the glasses have an inverse exponential relationship between solubility and CaO content. Furthermore, there is evidence for compositional related non-linearity in the dissolution of the glasses with time. This is thought to be due to either layer formation on the glass surface hindering ion diffusion, ion exchange process or change of ionic strength of the solution. Bioactivity of these glasses is indicated by the formation of a brushite precipitate, a precursor to apatite formation. Further evidence for bioactivity is also presented in the second part of this paper.

Journal Article↗

PubMed2000

Correlation between light intensity and exposure time on the hardness of composite resin.

This study evaluated the correlation between light intensity emitted by the curing units and exposure time on the of degree polymerization of dental composites by measured Knoop hardness. Specimens with 5 mm diameter and 2 mm height were prepared in a copper mold, covered with a mylar strip and polymerized for 30 sec by curing units with 50, 130, 180, 220, 280 and 520 mW/cm(2), respectively. The output for all units was measured using a Curing Radiometer (Demetron). Other specimens were polymerized for 45, 60, 75, 90, 105, 120, 135, 150, 165 and 180 sec utilizing units of 130, 220 and 280 mW/cm(2). Knoop hardness values of the top and bottom surfaces were measured after 24 h. The results indicate that the curing units with higher light intensity presented improved values of Knoop hardness on the top and bottom regions. As expected, the top surface always presented improved Knoop hardness values in relation to the bottom, after exposure for 30 sec. The values obtained on the surface were statistically superior compared to the values on the bottom (p<0.05) for the intensity of 130, 220 and 280 mW/cm(2) after 30, 45 and 60 sec of exposure.

Journal Article↗

PubMed2000

Influence of curing tip distance on composite Knoop hardness values.

The purpose of this paper was to study the influence of curing tip distance on Knoop hardness values, at different depths, of two composites, Z100 and Silux Plus. Specimens (5 mm in diameter and 2.5 mm in height) were prepared in a copper mold, covered with mylar strip and polymerized for 40 s, at 3 tip-to-composite surface distances: 0 mm (surface contact), 6 and 12 mm, utilizing an XL 3000 curing unit, with 750 mW/cm2 power. The specimens were then stored at 37 degrees C for 24 h. Knoop hardness values were measured using a microhardness tester, with a load of 50 g for 30 s for each indentation. Four specimens were made for each distance and composite and eighteen indentations were made of each specimen. The results were submitted to analysis of variance and Tukey test at 5% significance level. The results indicated that 1) composite Z100: the larger the curing tip distance in relation to the composite, the lower the Knoop hardness values; 2) Silux Plus: increasing the curing tip distance did not produce a statistically significant difference in the Knoop hardness values; however, at 6 and 12 mm, the deeper layers showed lower Knoop hardness values in relation to the surface; 3) Z100: statistically superior in relation to Silux Plus at all three curing tip distances and at all depths (P < 0.05).

Analysis of Variance↗

PubMed1999

Flow cytometry analysis of effects of glass on response of osteosarcoma cells to plasma-sprayed hydroxyapatite/CaO-P(2)O(5) coatings.

Multilayered coatings composed of mixtures of hydroxyapatite (HA) and P(2)O(5)-based bioactive glasses offer potential clinical benefits in orthopedic and dental surgery. In this study double-layer plasma-sprayed coatings were prepared and the biological response evaluated in tissue culture using two human osteosarcoma cell lines, MG63 and HOS TE85 (HOS). The cells were cultured on the materials and the effects on cell growth were determined using a spectrophometric assay of a mitochondrial enzyme that is active in viable cells. While none of the materials influenced the growth of the MG63 cells, the HOS cells appeared to undergo less proliferation on all the HA materials. Flow cytometry analysis was carried out using rabbit antibodies against osteonectin, osteopontin, bone sialoprotein, fibronectin, and collagen type I to measure the effects of the materials on key cellular functions. The results showed that the materials downregulated the expression of these extracellular matrix antigens by MG63 cells whereas they had less effect on the HOS cells compared to the same cells incubated on a plastic surface. Notably, with both cell lines the composite with the higher percentage of glass restored the production of connective tissue proteins to levels that were more similar to those present in the control cells.

Animals↗

PubMed1999

The biaxial flexural strength of two pressable ceramic systems.

The biaxial flexural strength of Optimal pressable ceramics and IPS Empress pressable ceramics were tested, compared and the micro-structures and compositions explored. The materials evaluated were Optimal shaded (Opcs) and unshaded (Opcus) ceramics and IPS Empress shaded (Ems) and unshaded (Emus) ceramics. Twenty-one disc specimens per material were prepared, heat-treated and tested. The piston on three-ball test ASTM F394-78 (1991) was used to test the specimens in a universal testing machine at a crosshead speed of 0.15 mm/min. Specimens were viewed in a scanning electron microscope and X-ray diffraction used to determine the phases present. Mean strengths (MPa +/- SD) were: Ems 120.1 +/- 20.5, Emus 135.8 +/- 16.0, Opcs 139.1 +/- 14.3 and Opcus 138.0 +/- 11.5. There was no statistically significant difference between Optimal shaded, Optimal unshaded and Empress unshaded strength values (p > 0.05). Empress shaded strength values were significantly lower than the other materials tested (p < 0.05). Weibull analysis provided m values: Ems 6.1, Emus 10.2, Opcs 12.8 and Opcus 13.9 and 1% and 5% probabilities of failure. Secondary electron imaging revealed a dense dispersal of leucite crystals in the glassy matrix of the Optimal ceramics of an average size 5.5 +/- 9.7 micron 2 for the Optimal shaded ceramic and 6.6 +/- 13.3 micron 2 for the Optimal unshaded ceramic. Leucite crystal agglomerates were evident for the Empress shaded material and a uniform distribution of fine leucite crystals (1.9 +/- 1.8 micron 2) for the Empress unshaded ceramic. Crystal and matrix microcracking were present in most of the material microstructures, together with porosity and tabular alumina platelets in the Optimal ceramics. X-ray diffraction revealed the presence of tetragonal leucite and small amounts of cubic leucite. Optimal ceramics and Empress unshaded ceramic provided higher strength and Weibull m values compared with Empress shaded ceramic. Inherent material defects were characterised and cubic leucite was identified.

Aluminum Silicates↗

PubMed1999

Effect of convergence angle and luting agent on the fracture strength of In ceram crowns.

This study compared the fracture strength of In ceram crown shapes fabricated with either 8 or 16 degrees total occlusal convergence; and attached with either a commercial zinc phosphate cement or a glass ionomer cement. Thirty crown shapes (8 mm diameter and 8.5 mm high) were fabricated for each preparation design on a brass master die with approximately the same dimensions as a premolar. In ceram crown shapes were luted on to the die using zinc phosphate or glass ionomer. The crown shapes were fractured in a testing machine (Instron) using a steel ball, 4 mm in diameter, that contacted the occlusal surface and the resulting data were statistically analyzed using a Mann-Whitney test. The results indicate that there is no statistical difference in the fracture strength values between preparations with 8 degrees total convergence compared with 16 degrees using the same cement. However, crown shapes luted with zinc phosphate on preparations with 8 and 16 degrees total occlusal convergence were significantly stronger than those luted using glass ionomer cements (p<0.05).

Journal Article↗

PubMed1998

Flow cytometry for assessing biocompatibility.

Flow cytometry (FCM) was examined as a possible procedure for measuring in vitro the biocompatibility of implant materials for orthopedic and dental surgery. The human osteoblast-like cell line MG63 was grown on hydroxyapatite (HA) and P2O5 glass-reinforced HA composite discs and compared with the same cells grown on polystyrene culture dishes. While morphological observation at the light and electron microscopic levels showed no major deleterious effects, FCM indicated that cell size was somewhat reduced, particularly by growth on the HA composite. Morever, this material also appeared to delay the progression of the cells from the G0/G1 into the S phase of the cell cycle. In addition to this low level of inhibition of cell growth relative to control cultures, FCM analysis also demonstrated that the glass-reinforced HA caused some down-regulation of the expression of osteocalcin and fibronectin, two antigens which play a vital part in the integrity and function of bone and soft connective tissue, respectively. These results thus show, first, that although HA and the HA composite used in these experiments were generally biocompatible, they nevertheless had certain suboptimal effects on the cells; and second, that FCM could be a highly useful procedure for effectively screening and evaluating important biological responses to implant materials.

Biocompatible Materials↗

PubMed1998

Glass-reinforced hydroxyapatite: a comprehensive study of the effect of glass composition on the crystallography of the composite.

Glass-reinforced HA composites were produced using phosphate-based glasses, and a structure refinement was carried out to determine the effect of the glass on the structure of the residual HA. Quantitative phase analysis showed that the glass causes some of the HA to decompose to beta-TCP and, at higher temperatures, to alpha-TCP. It also was indicated that when three phases were present, the formation of the alpha-TCP arose from decomposition of the beta-TCP and not from further decomposition of HA to alpha-TCP. The unit cell dimensions showed a decrease in the a axis and an increase in the c axis, giving an overall unit cell decrease in volume. There also was a significant effect based on the amount of glass added. The changes found in the composite containing the 4 wt% glass were attributed to the loss of carbonate and loss of hydroxyl. This was expected to cause shrinkage in the unit cell; however this was not seen, and therefore the major changes in the unit cell were attributed to the ions from the glass taking an interstitial role in the HA structure, thus not allowing the unit cell to shrink as much as expected.

Ceramics↗

PubMed1998

Analysis of in vitro reaction layers formed on Bioglass using thin-film X-ray diffraction and ATR-FTIR microspectroscopy.

Fourier transform infrared spectroscopy and thin-film X-ray diffraction (TF-XRD) techniques were used to analyze the inorganic carbonate apatite (CA) layer developed on a bioactive glass (45S5 type Bioglass) in an in vitro environment. The C-O and P-O vibrational modes appeared on the bioactive glass surface following immersion in the simulated body fluid solution. Initially, the C-O and P-O peaks increased with immersion time as crystallization of CA phase progressed. The TF-XRD confirmed that the deposited layer was apatite, crystallographically. Furthermore, evidence of preferred orientation in the 001 direction was seen, indicated by very strong 002 reflection. With time, the crystal growth became more random and the intensity of the 002 reflection decreased.

Biocompatible Materials↗

PubMed1998

Comparison of the wet and dry fatigue properties of all ceramic crowns.

The purpose of this paper was to investigate the influence of fatigue on the fracture strength of In ceram, optimal pressable ceramic (OPCTM) and IPS Empress in both wet and dry environments. Twenty-six crown shapes 8 mm in diameter and 8.5 mm in height were fabricated for each ceramic system. For each ceramic system, ten specimens were tested for fracture strength without fatiguing. The second group was submitted to a fatigue and fracture test in a dry (eight specimens) and a third group in a wet (eight specimens) environment using an Instron testing machine. The results were statistically analysed using a Mann-Whitney test. The results indicated that: (i) the fracture strength for In ceram was significantly stronger than OPCTM and IPS Empress (p<0.05) - no difference was found between OPCTM and IPS Empress; (ii) fatiguing and fracture testing showed a significant decrease in the fracture strength for In ceram and IPS Empress in the wet environment and no difference was found in the dry environment - no difference was found for OPCTM; and (iii) when fatigued in a dry environment, In ceram crown shapes were significantly stronger than OPCTM and IPS Empress (p<0.05) - the same statistical differences were found when fatigued in a wet environment.

Journal Article↗

PubMed1998

Fracture strength of all-ceramic crowns.

This paper compares the fracture strength of three types of all-ceramic crown shape systems (In ceram, OPC and IPS Empress) cemented with either a commercial resin cement, zinc phosphate or glass ionomer. Twenty test crown shapes with 8 mm diameter and 8.5 mm height were fabricated for each type of ceramic. Ten In ceram crown shapes were luted on the die using zinc phosphate, while ten OPCTM and IPS Empress were luted using resin cement specified for the particular system. Another ten specimens each, of In ceram, OPC and IPS Empress, were luted on the die using a glass ionomer. The crown shapes were fractured in a mechanical testing machine (Instron) using a steel ball, 4 mm diameter, that contacted the occlusal surface and the resulting data were statistically analysed using a Mann-Whitney test. The results showed that: (1) In ceram crown shapes luted with zinc phosphate were significantly stronger than IPS Empress crown shapes luted with resin cement (p < 0.05), but no difference was observed compared with OPC crown shapes luted with resin cement. No statistical difference was found between OPC and IPS Empress crown shapes. (2) When the three ceramics were luted with glass ionomer, the In ceram was significantly stronger than OPC (p < 0.05) and IPS Empress (p < 0.05). OPC was significantly stronger than IPS Empress (p < 0.05).

Journal Article↗

PubMed1997

Preparation and characterization of fluoride-substituted apatites.

Apatites were prepared with three different fluoride concentrations: 0.0 mM (pure hydroxyapatite) 2.5 mM and 5 mM. Reactions were performed in aqueous medium using a reaction between diammonium orthophosphate and calcium nitrate 4-hydrate and ammonium fluoride at temperatures of 3 degrees, 25 degrees, 60 degrees and 90 degrees C. The effects of reaction temperature and fluoride concentration on the crystal morphology, phase purity and crystallinity of the precipitates were observed, using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and ion chromatography. Transmission electron micrographs revealed that the crystallites precipitated at 3 degrees C were spheroidal, but became increasingly acicular with increasing precipitation temperature. X-ray diffraction results indicated that all the materials produced were phase pure and that the crystallinity of apatites prepared at higher precipitation temperatures was higher than those prepared at lower precipitation temperatures. A significant difference in the a-axis dimension of fluoride-substituted apatites was observed, as compared to hydroxyapatite. FTIR spectroscopy revealed a hydroxyl band at 3568 cm-1, along with a broad peak of adsorbed water in the region of 3568 cm-1 to 2670 cm-1 in the hydroxyapatite and fluoride-substituted apatite powders. Hence by careful selection of the precipitation conditions and fluoride contents, the composition and morphology of fluoride-substituted apatite may be controlled and this has interesting implications for the development of these materials for biomedical implantation.

Journal Article↗

PubMed1997

Structural analysis of calcium phosphate coatings produced by pulsed laser deposition at different water-vapour pressures.

Calcium phosphate coatings have been produced by pulsed laser deposition (PLD) at different water-vapour pressures. Rietveld refinement of X-ray diffraction (XRD) data allows us to determine that the structure of these coatings is apatitic with carbonate substitution for phosphate. The carbonate substitution decreases when the chamber pressure is raised, a fact that has been corroborated by Fourier transform-infrared (FT-IR) spectroscopy. Carbonate concentrations between 5 and 17 wt% have been calculated for the crystalline samples. Amorphous coatings are produced at the lowest and highest pressures due to the high carbonate concentration in the first case, and possibly to another type of substitution (Mg(2+), HPO(2-)4, P2O(4-)7) or the inherent kinetics of the PLD process, in the second case.

Journal Article↗

PubMed1996

Characterization of apatite layer formation on P2O5-CaO, P2O5-CaO-Na2O, and P2O5-CaO-Na2O-Al2O3 glass hydroxyapatite composites.

P2O5-based glass hydroxyapatite (HA) composites denoted HA-2 oxide, HA-3 oxide, and HA-4-oxide, were immersed in Hank's balanced salt solution for a period of 1, 2, 3, and 4 weeks at 37 degrees C in nonagitated condition for in vitro evaluation. A surface layer was precipitated on the composites that was analyzed using scanning electron microscopy (SEM), X-ray photoelecton spectroscopy, and thin film X-ray diffractometry (TF-XRD). SEM micrographs showed complete coverage of the composite surface by crystallites after immersion of 1 week in the solution, which grew thicker with respect to immersion time. The binding energies measured by XPS indicated apatite formation and the presence of carbonate on the composite surface, showing the newly formed layer was a carbonated apatite. Confirmation of the formed apatite layer was obtained by TF-XRD.

Glass↗

PubMed1996

Sintering effects in a glass reinforced hydroxyapatite.

Glass was incorporated into hydroxyapatite (HA) to act as a sintering aid in order to improve the mechanical properties. The glass was added at 2 and 4 wt% and the powders compacted uniaxially. The compacts were sintered at a variety of temperatures (1200, 1250, 1300 and 1350 degrees C) and the effects of the glass addition and the firing temperature were studied to determine their effects on the sintering process. It was found that the glass promoted some phase changes, related to the amount of glass added to the composite. At 1200 and 1250 degrees C, some beta-tricalcium phosphate (TCP) was found with the residual being HA. However, at 1300 and 1350 degrees C, both beta- and alpha-TCP were formed. The 4 wt% addition, as expected, promoted higher levels of secondary phases in the composite. The flexural bend strength (FBS) showed high values and also significant differences dependent on the amount of glass added. A 2 wt% addition gave a gradual increase in FBS with temperature. With a 4 wt% addition there was an increase in FBS, but above 1300 degrees C there was a rapid decrease. These effects were mirrored in the linear shrinkage. Both the linear shrinkage and the FBS results were attributed to both the phase changes occurring and also change in grain size with increasing firing temperature.

Chemical Phenomena↗