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At least 1,531 records · Page 85Linked to original sources
PubMed2005

Combined X-ray diffraction and diffuse reflectance analysis of nanocrystalline mixed Sn(II) and Sn(IV) oxide powders.

Nanocrystalline mixtures of Sn(II) and Sn(IV) oxide powders, potential gas sensor materials, are synthesized via a simple precipitation route using SnCl(2) as the precursor. Materials are characterized by powder X-ray diffraction, thermogravimetric analysis, UV-visible diffuse reflectance spectroscopy (DRS), and Fourier transform infrared spectroscopy. The ratio of Sn(II)/Sn(IV) in powders precipitated at room temperature, as well as the identity of the primary Sn(II) product (SnO or Sn(6)O(4)(OH)(4)), can be varied by adjusting aging time and washing procedures. The identity of the initial Sn(II) product influences the subsequent phase composition and degree of disorder in the tetragonal SnO(2) phase obtained following sintering in air. Analysis of the DRS absorption edge and long-wavelength (Urbach) absorption tail is used to determine the SnO(2) optical band gap and extent of disorder. SnO(2) obtained by heating the SnO/SnO(2) mixture at 600 or 800 degrees C has a smaller optical band gap and a broader Urbach tail than the analogous sample obtained from heating Sn(6)O(4)(OH)(4), indicating a more disordered material.

Crystallization↗
PubMed2003

In situ neutron diffraction studies of single crystals and powders during microwave irradiation.

Microwave dielectric heating has become an important method in chemical synthesis and materials processing over the past 15 years, and in the case of the reactions in solutions, there is a well-developed understanding of heating mechanisms and their influence on reaction rate. In the solid-state however, there is much less clarity, despite the advantages to be gained from better insight into the way in which such electromagnetic radiation may couple directly to charge carriers, accelerating reactions in good conductors. The related issue of the influence of microwave irradiation on biological systems, in particular, proteins, and the way in which this may pose hazards to health is similarly poorly understood despite the obvious relevance this may have to the current debate on the influence of electromagnetic radiation, in particular, microwave transmission, on human health. One reason for the paucity of fundamental insight in both fields is because most work has been performed with microwave equipment whose design is derived from that of a domestic oven, and which is not ideal for in situ studies of microwave driven processes. We have been developing new methods of irradiating a variety of solid samples while measuring structural parameters through a range of diffraction techniques, and describe apparatus that will enable X-ray or neutron scattering measurements to be performed on powders or single crystals under microwave irradiation with controlled power level. We also describe preliminary studies of a single crystal of the molecular solid aspirin, and a powder of the microwave-susceptible ionic material BaTiO3, during microwave irradiation.

Aspirin↗
PubMed2001

Gentamicin bone cements: characterisation and release (in vitro and in vivo assays).

Due to the extended use of acrylic bone cements, its necessary to develop improved formulations in order to resolve their many drawbacks. The present work was conducted to make a physical-chemical characterisation of this kind of acrylic cement in order to introduce future changes in the formulations to: (1) improve or at least maintain their mechanical properties; (2) diminish their toxicity, and (3) control the drug release (rate and amount). From the dissolution method we can conclude that the preparation method (with or without pressure) of specimens is not responsible for the erratic release. The cumulative amount of gentamicin released was fitted to a semi-empirical equation to explain the possible release mechanism. The powder size, shape and distribution that could affect several properties of bone cement were studied with the aid of different techniques such as SEM, laser diffraction spectroscopy, and powder X-ray diffraction. From SEM micrographs, it was possible to observe that the surfaces of the specimens were very irregular with numerous small craters that may serve as conduits for eluting the antibiotic. An 'in vitro' drug diffusion model is proposed to elucidate the drug release mechanism. Finally an 'in vivo' study was performed to evaluate the antibiotic release to the neighbouring bone sites.

Acrylic Resins↗
PubMed2003

Software for automatic calibration of synchrotron powder diffractometers.

An automatic procedure to calibrate angular-dispersive monochromatic diffraction instruments has been developed at the Daresbury Synchrotron Radiation Source. The procedure uses a macro Language to control the powder diffraction instruments to locate Bragg reflections and perform peak-centre refinement from a standard reference material. The information obtained is used to refine the wavelength of the radiation used and the angular offset of the detector arm. The concept and implementation of the new software are described with applications to demonstrate its viability. The results of a reliability and accuracy study are also presented.

Journal Article↗
PubMed2006

Particle design of three-component system for sustained release using a 4-fluid nozzle spray-drying technique.

We prepared composite particles of acetaminophen (Act) with chitosan (Cht) and hydroxypropylmethylcellulose phthalate (HPMCP) as a carrier using a newly developed 4-fluid nozzle spray-dryer. Cht dissolves in acid solutions and forms a gel, but it is insoluble in alkaline solutions. On the other hand, HPMCP is insoluble in acid solutions, but it dissolves in alkaline solutions. Therefore, we tested a preparation of controlled release composite particles using the characteristics of these carriers. Act and Cht mixtures in prescribed ratios were dissolved in an acid solution. Composite particles of Act and HPMCP in prescribed ratios were dissolved in alkaline solutions. We evaluated the composite particles of the three components (Act, Cht, and HPMCP) by preparing solid dispersions using a 4-fluid nozzle spray-dryer. Observation of particle morphology by scanning electron microscopy (SEM) revealed that the particles from the spray-drying process had atomized to several microns and had all become spherical. We investigated the physical properties of the composite particles by powder X-ray diffraction, differential scanning calorimetry, and dissolution rate analysis to clarify the effects of crystallinity on the dissolution rate. Powder X-ray diffraction peaks and the heat of fusion of Act in the spray-dried samples decreased in proportion to the carrier content, indicating that the drug was amorphous. These results indicate that the Act-Cht-HPMCP system formed a solid dispersion. Furthermore, we investigated the interaction between the drug and the carrier using FT-IR analysis. FT-IR spectroscopy of the Act solid dispersions suggested that the Act carbonyl and Cht amino groups formed a hydrogen bond. On the other hand, interaction by hydrogen bond was observed between the carbonyl group of HPMCP with the amino group of Act. In the three-component Act-Cht-HPMCP system, the 4-fluid nozzle spray-dried preparation with a mixing ratio of 1 : 2.5 : 2.5 obtained sustained release preparation in all pH test solutions.

Acetaminophen↗
PubMed2000

Whisker growth of l-menthol in coexistence with various excipients.

The purpose of the present study was to clarify the mechanism for l-menthol whisker growth. l-Menthol was mixed with an excipient, and the interaction was examined by IR measurement, thermal analysis and powder X-ray diffraction. Then we examined the involvement of the capillary condensation using the pore size distribution measurement. By mixing l-menthol with an excipient with whisker growth, the hydroxyl group stretching band of l-menthol was shifted to the higher wavenumber in the IR spectrum, the melting point and heat of fusion of l-menthol became lower in the thermal analysis, and the diffraction intensity of l-menthol became lower in the powder X-ray diffraction. The excipients with whisker growth showed the tendency to have the meso-pore involved in the capillary condensation in the pore size distribution measurement. From the above results, the whisker growth mechanism is considered as follows. When l-menthol was mixed with an excipient with whisker growth, the crystallinity of l-menthol was lowered and the vapor pressure was increased by the interaction mainly consisting of the hydrogen bond. The generated l-menthol vapor entered meso-pore, the saturated vapor pressure was lowered by the capillary condensation, and the nucleation occurred. The vapor was further supplied, generating the growth of whisker.

Crystallization↗
PubMed2002

Preformulation studies and characterization of proposed chondroprotective agents: glucosamine HCl and chondroitin sulfate.

PURPOSE: Glucosamine HCl and chondroitin sulfate are proposed chondroprotective agents commonly used as dietary supplements. This study examined the physicochemical and mechanical properties of chondroitin sulfate, glucosamine HCl powder, and glucosamine HCl granulation obtained from various sources. METHODS: The particle size distributions of the materials were determined using sieve analysis and time-of-flight techniques. Polarized light microscopy was used to examine particle morphology. Powder x-ray diffraction studies, moisture sorption isotherms, deformation behavior, powder flow, and compaction characteristics were also investigated. The polarized light microscopy and x-ray diffraction patterns showed that chondroitin sulfate is amorphous while glucosamine HCl is crystalline. Particle sizes of chondroitin sulfate and glucosamine HCl varied widely, depending on their source or manufacturing technique (e.g., granulation). The studied samples of shark-derived chondroitin sulfate had a small median particle size (4 microns) compared to that derived from bovine cartilage (17 microns). Different moisture sorption profiles were obtained for the glucosamine HCl granulations studied. Glucosamine HCl granulation from Supplier I showed no observable moisture sorption, while the granulation from Supplier II showed an approximately 5% weight gain. Conversely, chondroitin sulfate was extremely hygroscopic and deliquescent. The Carr's indices for glucosamine HCl samples ranged from 12.5 to 31.5; for chondroitin sulfate the values were 25.2 and 53.6. The compression analysis showed that all chondroitin sulfate samples exhibited plastic deformation behavior, with the shark-derived chondroitin sulfate forming superior compacts when compared to the bovine. The dominant mechanism of compression of glucosamine HCl powder was brittle fracture, whereas wet granulated glucosamine HCl exhibited plastic deformation with enhanced mechanical strength. CONCLUSIONS: The physicochemical and mechanical characteristics between the various dietary supplements studied varied greatly. Data obtained from this study provide an understanding of the physicomechanical behavior of chondroitin sulfate and glucosamine HCl. Application of this knowledge would facilitate development of stable solid dosage forms containing these materials.

Animals↗
PubMed2004

Incommensurate magnetic ordering in Cu2Te2O5X2 (X = Cl,Br) studied by neutron diffraction.

We present the results of the first neutron powder and single crystal diffraction studies of the coupled spin tetrahedra systems Cu2Te2O5X2 (X = Cl,Br). Incommensurate antiferromagnetic order with the propagation vectors kCl approximately [0.150,0.422,1/2], kBr approximately [0.158,0.354,1/2] sets in below TN = 18 K for X = Cl and 11 K for X = Br. No simple collinear antiferromagnetic or ferromagnetic spin arrangements within Cu2+ tetrahedra fit these observations. Fitting the diffraction data to more complex but physically reasonable models with multiple helices leads to a moment of 0.67(1)microB/Cu2+ at 1.5 K for the Cl compound. The reason for such a complex ground state may be geometrical frustration of the spins due to the intratetrahedral and intertetrahedral couplings having similar strengths. In neither compound has any evidence for a structural transition accompanying the magnetic ordering been found.

Journal Article↗
PubMed2006

Characterisation of a carrier-free dry powder aerosol formulation using inertial impaction and laser diffraction.

PURPOSE: The purpose of the study was to examine the suitability of using laser diffraction to measure the fine particle fraction (FPF) of drugs emitted from carrier-free dry powder aerosol formulations. MATERIALS AND METHODS: Particle size distribution of terbutaline sulphate from Bricanyl Turbohaler, which contained loose agglomerates of drug particles only, was measured separately by laser diffraction apparatus equipped with a metal throat and a twin-stage, multi-stage liquid impingers, or Andersen cascade impactor at flow rates ranging from 28.3 to 100 l min(-1). In-line measurements were then conducted which allowed the same aerosolised particles to be measured first by laser diffraction then captured by an impactor or impinger for subsequent chemical analysis. RESULTS: A significant linear correlation (p < 0.001, R2 = 0.96, ANOVA) existed between the results obtained from two techniques when measurements were conducted independently. There was little difference in FPFs measured by inertial impaction and laser diffraction at the same flow rate. When in-line measurements were conducted, the FPFs measured by inertial impaction were approximately 0.7-0.9 times the aerosol FPFs measured by laser diffraction. This linear relationship was statistically significant and had a statistically insignificant y-intercept, regardless of inhaler batches, impinger types and measuring position of the laser beam. CONCLUSION: Laser diffraction could prove to be a reliable technique for development, evaluation and quality control of carrier-free, dry powder aerosol formulations.

Aerosols↗
PubMed1981

Dissolution, stability, and absorption characteristics of dicumarol in polyethylene glycol 4000 solid dispersions.

The dissolution characteristics of dicumarol were markedly enhanced by preparing dispersions of drug in polyethylene glycol 4000. Solid dispersions of varying weight fractions were formed by a melt method without measurable drug degradation or evaporation. There were no significant differences in dissolution rates among weight fractions, with dynamic solubilities being approximately 2.5 times greater than dicumarol's equilibrium solubility. No indications of drug polymer complexation were noted from equilibrium or in situ absorption experiments. Incorporation of solid dispersions into direct compression tablets provided dosage forms with fast-release properties relative to test tablets of physical mixtures and a commercially available product. Percentages dissolved in 30 min were 370% greater for 1:3 and 1:5 (w/w) solid dispersion tablets compared to a commercial tablet at 37 degrees with a pH 7.5 dissolution buffer. X-ray diffraction of test powder revealed that the crystalline nature of the drug had altered during fusion preparation. Dissolution traits and drug stability for solid dispersions were maintained over 1 year of storage.

Absorption↗
PubMed2005

Hydrogen cycling of niobium and vanadium catalyzed nanostructured magnesium.

The reaction of hydrogen gas with magnesium metal, which is important for hydrogen storage purposes, is enhanced significantly by the addition of catalysts such as Nb and V and by using nanostructured powders. In situ neutron diffraction on MgNb(0.05) and MgV(0.05) powders give a detailed insight on the magnesium and catalyst phases that exist during the various stages of hydrogen cycling. During the early stage of hydriding (and deuteriding), a MgH(1< x < 2) phase is observed, which does not occur in bulk MgH(2) and, thus, appears characteristic for the small particles. The abundant H vacancies will cause this phase to have a much larger hydrogen diffusion coefficient, partly explaining the enhanced kinetics of nanostructured magnesium. It is shown that under relevant experimental conditions, the niobium catalyst is present as NbH(1). Second, a hitherto unknown Mg-Nb perovskite phase could be identified that has to result from mechanical alloying of Nb and the MgO layer of the particles. Vanadium is not visible in the diffraction patterns, but electron micrographs show that the V particle size becomes very small, 2-20 nm. Nanostructuring and catalyzing the Mg enhance the adsorption speed that much that now temperature variations effectively limit the absorption speed and not, as for bulk, the slow kinetics through bulk MgH(2) layers.

Catalysis↗
PubMed1989

Effects of the mechanical energy of multi-tableting compression on the polymorphic transformations of chlorpropamide.

The effects of the mechanical energy of tableting compression on the polymorphic transformation of chlorpropamide have been examined. A single-punch eccentric tableting machine with a load cell and a non-contact displacement transducer were used to measure compression stress, distance and energy. An amount of 100 mg of the stable form A or the meta-stable form C of the drug was loaded into the press and the sample compressed with a compression stress of 196 MPa at room temperature (20 degrees C). The compression cycle was repeated from 1 to 30 times. The powder X-ray diffraction profiles of the deagglomerated compressed sample powder were measured to calculate the polymorphic content. The results on forms A and C suggested that both forms were transformed into each other in the solid state by mechanical energy during tableting. The contents of forms A and C reached equilibrium at a constant value above 100 J g-1 of compression energy after more than 10 cycles. After 30 tableting cycles of forms A and C, the contents of A, C and the non-crystalline solid were almost constant at about 45, 25 and 30%, respectively. The compression energies were estimated to be about 500-600 J g-1. From the results it seems that the transformation mechanism of forms A and C during tableting were as follows. The crystal form of A or C was converted to a non-crystalline solid by the mechanical energy, and the solid was then transformed into form A or C.

Chemical Phenomena↗
PubMed2006

Structures, photoluminescence, and reversible vapoluminescence properties of neutral platinum(II) complexes containing extended pi-conjugated cyclometalated ligands.

Reacting K2PtCl4 with the tridentate R-C(wedge)N(wedge)C-H2 ligands 2,6-di-(2'-naphthyl)-4-R-pyridine (R = H, 1a; Ph, 1b; 4-BrC6H4, 1c; 3,5-F2C6H3, 1d) in glacial acetic acid, followed by heating in dimethyl sulfoxide (DMSO), gave complexes [(R-C(wedge)N(wedge)C)Pt(DMSO)] (2a-d). In the crystal structures of 2a-c, the molecules are paired in a head-to-tail orientation with Pt...Pt separations >6.3 A, and there are extensive close C-H...pi (d = 2.656-2.891 A), pi...pi (d = 3.322-3.399 A), and C-H...O=S (d = 2.265-2.643 A) contacts. [(Ph-C(wedge)N(wedge)C)Pt(PPh3)] (3) was prepared by reacting 2b with PPh3. Reactions of 2a-d with bis(diphenylphosphino)methane (dppm) gave [(R-C(wedge)N(wedge)C)2Pt2(mu-dppm)] (4a-d). Both head-to-head (syn) and head-to-tail (anti) conformations were found for 4a.6CHCl3.C5H12, whereas only one conformation was observed for 4b.2CHCl3 (syn), 4c.3CH2Cl2 (syn), and 4d.2CHCl3 (anti). In the crystal structures of 4a-d, there are close intramolecular Pt...Pt contacts of 3.272-3.441 A in the syn conformers, and long intramolecular Pt...Pt separations of 5.681-5.714 A in the anti conformers. There are weak C-H...X (d = 2.497-3.134 A) and X...X (X = Cl or Br; d = 2.973-3.655 A) interactions between molecules 4a-d and occluded CHCl3/CH2Cl2 molecules, and their solvent channels are of varying diameters (approximately 9-28 A). Complexes 2a-d, 3, and 4a-d are photoluminescent in the solid state, with emission maxima at 602-643 nm. Upon exposure to volatile organic compounds, 4a shows a fast and reversible vapoluminescent response, which is most intense with volatile halogenated solvents (except CCl4). Powder X-ray diffraction analysis of desolvated 4a revealed a more condensed molecular packing of syn and anti complexes than crystal 4a.6CHCl3.C5H12.

Cyclization↗
PubMed2006

[Optimisation of the conditions of particle sizing of gentamicin sulfate].

One of the problems for the development of dry powder inhalation preparations is evaluation of particle size distribution of obtained micronized powders for the determination of theoretical aerodynamic diameter of the particles. The final aim of our study is the development of inhalation dry powder formulation of gentamicin sulfate, therefore it is necessary to determine theoretical aerodynamic diameter of micronized gentamicin sulfate particles. Micronized gentamicin sulfate powders are very cohesive and do not have satisfactory flow properties, the shape of the particles is close to spherical. The most suitable technique for this kind of powders is laser diffraction. On the basis of realized experiments the optimal conditions for the determination of particle size distribution of gentamicin powders were found. Results are in accordance with the data obtained by method-reference (Electron Microscopy).

Administration, Inhalation↗
PubMed2006

A novel white film for pharmaceutical coating formed by interaction of calcium lactate pentahydrate with hydroxypropyl methylcellulose.

We have found that a white film forms on tablets when a coating solution consisting of hydroxypropyl methylcellulose (HPMC), polyethylene glycol (PEG 6000) and calcium lactate pentahydrate (CLP) is used. The white film has also been found in casting film consisting of HPMC and CLP, and the surface state of coated tablets has been shown to be strongly affected by addition of PEG 6000. The aim of the present study was to investigate the mechanism of formation of this white film in order to derive an appropriate film prescription. Interaction among the base ingredients of the film was investigated using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and Fourier transform-infrared (FT-IR) spectroscopy. The casting film formed with HPMC and a large excess of PEG 6000 was found to be crystalline in form. In contrast, the amorphous film consisting of HPMC, PEG 6000 and excess CLP exhibited the crystallinity film by an excess addition of CLP. Although the crystalline film had many cracks, the amorphous film appeared to be excellent as a tablet coating. The most probable interaction sites between HPMC and CLP were demonstrated by FT-IR analysis of casting films consisting of HPMC, CLP and PVP.

Calcium Compounds↗
PubMed2005

The physicochemical characteristics of freeze-dried scutellarin-cyclodextrin tetracomponent complexes.

In an effort to improve the solubility of the insoluble drug scutellarin, a novel complexation of scutellarin with beta-cyclodextrin (beta-CD) was studied. Tetracomponent freeze-dried complex was prepared with scutellarin, beta-CD, Hydroxypropyl Methylcellulose (HPMC), and triethanolamine. To confirm complex formation, complex was characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction, and differential scanning calorimetry (DSC). Phase-solubility analysis suggested the soluble complexes having 1:1 stoichiometry. The beta-CD solubilization of scutellarin could be improved significantly by combining water-soluble polymer and pH adjuster. Comparing the binary, ternary solid systems with tetrary systems, tetracomponent freeze-dried complex showed the best effect of solubilization. A maximal solubility of scutellarin (23.65 mg/ml) was achieved with tetracomponent freeze-dried complex, up to 148-fold increase over scutellarin solubility in water, and the solubility of scutellarin is 15.35 microg/ml (up to 6-fold) in simulated gastric fluid.

Apigenin↗