Formation of nanosized strontium substituted hydroxyapatites

Incorporation of specific elements into calcium phosphates offers the combination of a bioactive material and a therapeutic effect. This is important for improving the integration of implants as well as treating medical conditions. Strontium is a suitable candidate and displays the ability to stimulate bone growth and reducing bone resorption. This study investigated the formation of strontium carbonated hydroxyapatite nanoparticles from an amorphous phase. Crystallization of carbonated hydroxyapatite occurred at 585 oC, but samples with an intended 25% and 75% replacement of calcium with strontium crystallized at 624 oC. Heat treatment at the crystallization temperature revealed that strontium free apatite does not crystallize in 5 minutes, but an increasing strontium concentration leads to a higher rate of crystallization. X-ray diffraction patterns suggest that it may be difficult to include strontium, but higher strontium concentrations are possibly included with ease in the lattice. This work has produced a nanosized apatite accompanied by an amorphous phase after a short heat-treatment time. This offers a range of features that collectively show great promise for significantly enhancing the release of strontium for improved bone therapeutic effects

Comparative study of conversion of coral with ammonium dihydrogen phosphate and orthophosphoric acid to produce calcium phosphates

© 2014, Australasian Ceramic Society. All rights reserved. Biogenic materials like corals, which are readily available, could be used to produce bioceramic materials and address significant advantages due to their unique structures and chemical compositions that contain Mg and Sr. Many conversion processes has been in the past proposed. In this work, a comparison study between the conversion of coral with orthophosphoric acid and ammonium dihydrogen phosphate was conducted. The resultant structures and compositions were studied using XRD, ICP-MS, SEM and FTIR. The results show that with phosphoric acid the coral was converted into mainly monetite (92%). The ammonium dihydrogen phosphate converted approximately 76% of the coral to hydroxyapatite through solid state reactions. The two routes proved to be effective in producing bioceramic materials from corals under moderate conditions of temperature with a basic condition favouring the yield of hydroxyapatite

Comparative study of coral conversion, Part 2: Microstructural evolution of calcium phosphate

© 2015, The Australian Ceramic Society. Calcium phosphate materials can be easily produced by a number of wet chemical methods that involve both acidic and basic environments. In our previous study, we investigated calcium phosphates such as monetite (DCPA), hydroxyapatite (HAp) and whitlockite which were successfully produced by mechano-chemical method from corals obtained from the Great Barrier Reef. It was observed that a number of synthesis factors such as the pH of the environment, the reaction temperature and the chemistry influenced the crystal size formed. A number of theories have been suggested on the mechanisms of crystal formation; however, very few mechanisms have been universally accepted. The present work was aimed to explore the evolution of crystalline calcium phosphate and their morphology with respect to the pH of the environment and reaction time. Conversion of coral to calcium phosphates was carried out with stoichiometric amount of required H3PO4 or (NH4)2HPO4, to obtain hydroxyapatite or tricalcium phosphate (TCP) phases. The acidic or basic solution was added, drop wise, at a rate of 2 mL min-1, to 6 g of coral powder suspended in 300 mL of distilled water at 80 ± 0.5°C on a hot plate with magnetic stirrer. The pH of reaction was monitored. Crystal morphology and the phases were identified by XRD, FTIR, and SEM studies. It was observed that under acidic conditions (H3PO4), dissolution and then precipitation influences the crystal morphology and transition from plate like to rod like hydroxyapatite structure. During the first hour of the dissolution a monetite and hydroxyapatite mixture precipitates and then the full conversion to hydroxyapatite is observed. However under basic conditions (NH4)2HPO4), pH is only marginally changed within the environment and just surface conversion of the calcium carbonate structure of coral to hydroxyapatite and a very small amount of tri-calcium phosphate is observed. The mechanism can be classified as the solid state topotactic ion-exchange reaction mechanism

Modern microwave methods in solid state inorganic materials chemistry: from fundamentals to manufacturing

No abstract available

Drug Facilitated Sexual Assault: Detection and Stability of Benzodiazepines in Spiked Drinks Using Gas Chromatography-Mass Spectrometry

Benzodiazepines are detected in a significant number of drug facilitated sexual assaults (DFSA). Whilst blood and urine from the victim are routinely analysed, due to the delay in reporting DFSA cases and the short half lives of most of these drugs in blood and urine, drug detection in such samples is problematic. Consideration of the drinks involved and analysis for drugs may start to address this. Here we have reconstructed the ‘spiking’ of three benzodiazepines (diazepam, flunitrazepam and temazepam) into five drinks, an alcopop (flavoured alcoholic drink), a beer, a white wine, a spirit, and a fruit based non-alcoholic drink (J2O) chosen as representative of those drinks commonly used by women in 16–24 year old age group. Using a validated GC-MS method for the simultaneous detection of these drugs in the drinks we have studied the storage stability of the benzodiazepines under two different storage conditions, uncontrolled room temperature and refrigerator (4°C) over a 25 day period. All drugs could be detected in all beverages over this time period. Diazepam was found to be stable in all of the beverages, except the J2O, under both storage conditions. Flunitrazepam and temazepam were found not to be stable but were detectable (97% loss of temazepam and 39% loss of flunitrazepam from J2O). The recommendations from this study are that there should be a policy change and that drinks thought to be involved in DFSA cases should be collected and analysed wherever possible to support other evidence types

Comparison of Physical-chemical and Mechanical Properties of Chlorapatite and Hydroxyapatite Plasma Sprayed Coatings

Chlorapatite can be considered a potential biomaterial for orthopaedic applications. Its use as plasma-sprayed coating could be of interest considering its thermal properties and particularly its ability to melt without decomposition unlike hydroxyapatite. Chlorapatite (ClA) was synthesized by a high-temperature ion exchange reaction starting from commercial stoichiometric hydroxyapatites (HA). The ClA powder showed similar characteristics as the original industrial HA powder, and was obtained in the monoclinic form. The HA and ClA powders were plasma-sprayed using a low-energy plasma spraying system with identical processing parameters. The coatings were characterized by physical-chemical methods, i.e. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy, including distribution mapping of the main phases detected such as amorphous calcium phosphate (ACP), oxyapatite (OA), and HA or ClA. The unexpected formation of oxyapatite in ClA coatings was assigned to a side reaction with contaminating oxygenated species (O2, H2O). ClA coatings exhibited characteristics different from HA, showing a lower content of oxyapatite and amorphous phase. Although their adhesion strength was found to be lower than that of HA coatings, their application could be an interesting alternative, offering, in particular, a larger range of spraying conditions without formation of massive impurities.This study was carried out under a MNT ERA-Net Project named NANOMED. The authors gratefully thank the Midi-Pyrénées region (MNT ERA Net Midi-Pyrénées Région, NANOMED2 project) and the Institute National Polytechnique de Toulouse (BQR INPT 2011, BIOREVE project) for supporting this research work, especially the financial support for research carried out in the CIRIMAT and the LGP laboratories (France), and the Basque government and Tratamientos Superficiales Iontech, S.A. for their financial and technical support under the IG-2007/0000381 grant for the development of the LEPS device and deposition of the coatings carried out in Inasmet-Tecnalia. The French industrial collaborators (TEKNIMED SA and 2PS SA) were financed by the OSEO programs

Glycosylation of Erythrocyte Spectrin and Its Modification in Visceral Leishmaniasis

Using a lectin, Achatinin-H, having preferential specificity for glycoproteins with terminal 9-O-acetyl sialic acid derivatives linked in α2-6 linkages to subterminal N-acetylgalactosamine, eight distinct disease-associated 9-O-acetylated sialoglycoproteins was purified from erythrocytes of visceral leishmaniaisis (VL) patients (RBCVL). Analyses of tryptic fragments by mass spectrometry led to the identification of two high-molecular weight 9-O-acetylated sialoglycoproteins as human erythrocytic α- and β-spectrin. Total spectrin purified from erythrocytes of VL patients (spectrinVL) was reactive with Achatinin-H. Interestingly, along with two high molecular weight bands corresponding to α- and β-spectrin another low molecular weight 60 kDa band was observed. Total spectrin was also purified from normal human erythrocytes (spectrinN) and insignificant binding with Achatinin-H was demonstrated. Additionally, this 60 kDa fragment was totally absent in spectrinN. Although the presence of both N- and O-glycosylations was found both in spectrinN and spectrinVL, enhanced sialylation was predominantly induced in spectrinVL. Sialic acids accounted for approximately 1.25 kDa mass of the 60 kDa polypeptide. The demonstration of a few identified sialylated tryptic fragments of α- and β-spectrinVL confirmed the presence of terminal sialic acids. Molecular modelling studies of spectrin suggest that a sugar moiety can fit into the potential glycosylation sites. Interestingly, highly sialylated spectrinVL showed decreased binding with spectrin-depleted inside-out membrane vesicles of normal erythrocytes compared to spectrinN suggesting functional abnormality. Taken together this is the first report of glycosylated eythrocytic spectrin in normal erythrocytes and its enhanced sialylation in RBCVL. The enhanced sialylation of this cytoskeleton protein is possibly related to the fragmentation of spectrinVL as evidenced by the presence of an additional 60 kDa fragment, absent in spectrinN which possibly affects the biology of RBCVL linked to both severe distortion of erythrocyte development and impairment of erythrocyte membrane integrity and may provide an explanation for their sensitivity to hemolysis and anemia in VL patients

Texture of alumina by neutron diffraction and SEM-EBSD

peer reviewedThe orientation distributions of alpha-Al2O3 textured ceramics are determined from neutron diffraction and SEM-EBSD. A curved position-sensitive detector coupled to a tilt angle (chi) scan allowed the whole neutron diffraction pattern treatment in the combined Rietveld-WIMV-Popa algorithm. Analyses from neutron and electron diffraction data gave similar results if EBSD data are smoothed to account for grain statistics. Four textured alumina ceramics were prepared by slip-casting under a high magnetic field and sintered at 800 degrees C, 1300 degrees C, 1400 degrees C and 1600 degrees C. The inverse pole figures and EBSD-mapping highlights the influence of the magnetic field and sintering temperature on the texture development. The inverse pole figures calculated for the fiber direction show a major (001) component for all the samples. With the increasing sintering temperature, the texture strength is enhanced and the c-axis distribution is sharper. The effectiveness of the combined approach for determining the crystallite size is also evident. As a global trend, the calculated crystallite size and observed grain size are similar and increase with the increasing sintering temperature. The mechanism of the texture development in the sintered specimens is certainly initiated from the preferred orientation of the green body after slip-casting under a high magnetic field. The basal texture is enhanced during sintering by selective anisotropic grain growth. We evidenced here the powerfulness of the Rietveld texture analysis correlated to SEM-EBSD calculation to provide a basis for the correlation of texture, microstructural parameters and anisotropic properties