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Crystallization, fluoridation and some properties of apatite thin films prepared through rf-sputtering from CaO-P2O5 glasses.

Using calcium phosphate glass targets with the CaO/P2O5 molar ratios of 1.50-0.50, much lower than the stoichiometric value of 3.3 for hydroxyapatite, thin films of stoichiometric hydroxy-, nonstoichiometric oxyhydroxy- and Ca-deficient oxyhydroxy-apatites were prepared on alumina ceramic substrates by rf-sputtering followed by post-annealing. Based on the present results, a phase diagram for CaO-P2O5 at low temperatures in the ambience of air was depicted for thin films. The ambient H2O vapor had an influence on the phase diagram: Tricalcium phosphate was changed to apatite in the presence of H2O vapor. Dense fluorohydroxyapatite thin films were prepared by fluoridation of those apatite thin films at a low temperature such as 200 degrees C. In the present report, some functional properties of thin films thus prepared were also shown.

Aluminum Oxide↗

On the synthesis of a 32P-labelled Edman reagent for the sensitive identification of amino-acid derivatives.

A phosphorus-32 containing derivative of phenylisothiocyanate was prepared to increase the sensitivity of amino-acid sequence determination. The respective compound 2-(4-isothiocyanatophenoxy)-1,3,2-dioxaphosphinane 2-oxide showed about the same reactivity, stability, and polarity as the Edman reagent itself. A repetitive yield of 94% was obtained in the stepwise degradation of insulin B chain using a solid phase sequencer. The synthesis of this radioactive reagent was achieved within 5 h but with a specific activity of 1 Ci/mol. Eight amino acids were reacted with the 32P-labelled reagent and identified by autoradiography after two dimensional thin-layer chromatography.

Amino Acid Sequence↗

Calcium phosphate formation on porous sol-gel-derived SiO2 and CaO-P2O5-SiO2 substrates in vitro.

Sol-gel-derived SiO2 and CaO-P2O5-SiO2 have been shown to be bioactive and bone bonding. In this study bioactive sol-gel-derived SiO2 and CaO-P2O5-SiO2 systems were tested for in in vitro bioactivity. The calcined ceramic monoliths were immersed in a simulated body fluid and analyzed to follow the hydroxyapatite formation on the ceramic surface. Apatite-forming ability was investigated in terms of structural changes by changing the composition and the preparation method. The role of Ca and P dopants in the substrate structure is complicated, and careful characterization is needed. The composition and structure together determine the in vitro bioactivity. The pore structure was analyzed using N2-adsorption/desorption isotherms. The results indicate that a great mesopore volume and a wide mesopore size distribution favor hydroxycarbonate apatite nucleation and a great surface area is not needed. The performed preparation process for silica in a basic environment provides a convenient way to prepare a mesoporous material.

Adsorption↗

Preparation and in vitro bioactivity of hydroxyapatite/solgel glass biphasic material.

Hydroxyapatite/solgel glass biphasic material has been obtained in order to improve the bioactivity of the hydroxyapatite (OHAp). A mixture of stoichiometric OHAp and the precursor gel of a solgel glass, with nominal composition in mol% CaO-26, SiO2-70, P205-4, has been prepared. The amounts of components used have been selected to obtain a final relationship for OHAp/solgel glass of 60/40 on heating. Two different thermal treatments have been used: (i) 700 degrees C, temperature of solgel glass stabilisation and (ii) 1000 degrees C, lower temperature of hydroxyapatite sintering. The bioactivity of the resulting materials has been examined in vitro by immersion in simulated body fluid at 37 degrees C. The results obtained show that both materials are bioactive. The apatite-like layer grown is greater for the new materials than for the OHAp and the solgel glass themselves.

Calcium Compounds↗

Optimisation of the selectivity of a pulsed flame photometric detector for unknown compound screening.

Identification of traces of chemical warfare agents (CWA) is generally performed with spectral methods such as mass spectrometry (MS) or NMR, but the use of element-specific detectors is most often required to extract interesting signals from gas chromatographic (GC) data heavily masked by natural interferents. The pulsed flame phosphorus detector (P-FPD) is able to detect phosphorus, sulphur and arsenic, and thus should be very well-suited to CWA detection. However, first results using standard operating conditions recommended by the manufacturer of P-FPD led to false positive detection of phosphorus-containing compounds on the sulphur line. Therefore, an optimisation process of the selectivity of P-FPD for phosphorus versus sulphur or arsenic was undertaken, and allowed to identify gate delay and gate width as crucial parameters for the performance of P-FPD. While selectivity could be significantly improved, unexpectedly, this resulted in a concurrent important loss of sensitivity (ca. 45%) for arsenic, which suggests that this detector should be carefully optimised with respect, and prior to its purported use.

Arsenic↗

Development and in vitro characterization of sol-gel derived CaO-P2O5-SiO2-ZnO bioglass.

A CaO-P(2)O(5)-SiO(2)-ZnO bioglass was formed by the sol-gel technique and characterized by Raman spectroscopy, X-ray diffraction, energy dispersive X-ray analysis (EDXA) and scanning electron microscopy (SEM). The surface reactivity of the resultant glass-ceramic specimens was analyzed by immersion studies in simulated body fluid (SBF). SEM-EDXS and inductively coupled plasma atomic emission spectrometry techniques were used to monitor changes in the glass surface and SBF composition. Osteoblast cell culture experiments were performed to assess the biocompatibility and the alkaline phosphatase activity. Cell counts of the osteoblasts cultured on the bioglass samples were studied and compared with the polystyrene plates. The cells cultured on the bioglass disks consistently showed a higher alkaline phosphatase activity and cell counts compared to cells cultured on either polystyrene plates or the base CaO-P(2)O(5)-SiO(2) bioglass. This was due to cell proliferation and differentiation promoted by the zinc-substituted bioglass.

Animals↗

In vivo MR spectroscopic imaging with P-31. Work in progress.

Magnetic resonance imaging techniques were applied to in vivo spectroscopic analysis of spatially resolved phosphorus spectra in the cat brain to determine whether changes associated with stroke could be detected. Two-dimensional images of separate phosphorus-containing compounds, as well as spectra arising from spatially localized points, demonstrated that metabolism within tissue could be monitored in this manner. Preliminary results of phosphorus imaging of the human body in vivo are reported.

Animals↗

Simultaneous accumulation of calcium, phosphorus, and magnesium in various human arteries.

To elucidate compositional changes of the arteries with aging, the authors investigated the relationships among average contents of calcium, phosphorus, sulfur, and magnesium in the arteries by inductively coupled plasma-atomic emission spectrometry. The arteries used were the thoracic and abdominal aortas, coronary, common carotid, anterior, middle and posterior cerebral, vertebral, basilar, internal thoracic, axillary, radial, truncus celiacus, common, internal and external iliac, femoral, popliteal, and umbilical arteries. It was found that high correlations were found between the average contents of calcium and phosphorus, between the average contents of calcium and magnesium, and between the average contents of phosphorus and magnesium in the arteries, but not between the average contents of sulfur and the other elements. These correlations revealed that as the content of calcium and phosphorus increased in the arteries, the magnesium content increased simultaneously in the arteries, but the sulfur content did not. It is likely that magnesium forms compounds with phosphorus in the arteries.

Adult↗