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At least 1,621 records · Page 90Linked to original sources
PubMed1999

Physico-chemical characterization of interactions between erythromycin and various film polymers.

In this study the interactions between erythromycin and various polymers (Eudragit L100, shellac, polyvinyl acetate phthalate (PVAP), cellulose acetate phthalate (CAP), hydroxypropyl methylcellulose acetate phthalate (HPMCP), and hydroxypropyl methylcellulose (HPMC)) were investigated. The polymer films containing drugs were prepared and characterized by the use of infrared spectroscopy, powder X-ray diffraction analysis, thermal analysis, thin layer chromatography, and nuclear magnetic resonance (NMR) spectroscopy. Preliminary studies of pure drug powders recrystallized in various organic solvent systems suggested a mixture of amorphous and crystalline forms whereas those recrystallized in water and organic solvent-water mixture led to the dihydrate form. Erythromycin in drug-polymer mixtures exhibited molecular dispersions in all six polymers studied. The amine salt interaction between the carboxyl group of the acid polymers and N-atom of erythromycin was indicated by the NMR technique. The solid solution of erythromycin in all polymer films studied was physically stable under stress conditions (8 degrees C/3 days and 40 degrees C/3 days for six cycles).

Anti-Bacterial Agents↗
PubMed1989

The crystallinity of human deciduous teeth in hypophosphataemic vitamin D-resistant rickets.

Five teeth were obtained from three patients with hypophosphataemic vitamin D-resistant rickets (HVDRR) and five corresponding sound teeth from five healthy children. According to powder X-ray diffraction analysis, the half-peak breadths of (310) and (002) reflections of HVDRR dentine were smaller than those of normal dentine. Splitting fractions obtained from i.r. spectral analysis of HVDRR dentine powder were larger than those of normal. Microbeam X-ray diffraction analysis showed that the relative half-peak breadths of globular dentine in ground sections of HVDRR teeth were smaller than those of normal circumpulpal dentine. Transmission electron microscopy demonstrated that the hydroxyapatite crystals of globular dentine in HVDRR teeth were larger than those of normal dentine. Thus the crystallinity of deciduous tooth dentine in HVDRR was greater than that of normal dentine, mainly because of the large hydroxyapatite crystals in HVDRR globular dentine.

Child↗
PubMed2003

Structural properties of magnesium stearate pseudopolymorphs: effect of temperature.

A thorough review of the relevant literature reveals that the interaction between water vapour and magnesium stearate, in contrast to many other metal soaps, is not properly understood. The structural modifications associated with the up-take or loss of water of vegetable-derived commercial magnesium stearate powders exposed to humid air or vacuum at room temperature are investigated using standard powder X-ray diffractometry. It is found that in such conditions magnesium stearate reacts reversibly with the vapour phase with structural consequences very similar to the high temperature transition between the crystalline and rotator phases of other anhydrous metal soaps. When temperature is increased under dry nitrogen the diffraction band characteristic of the rotator phase shifts towards higher angle values and the corresponding lattice spacing increases at the rate of 6.9x10(-4)C(-1). Melting takes place gradually above 100 degrees C as revealed by the collapse of the diffraction band and the growth of the broader diffusion band characteristic of the liquid state. Full clarification of the structure of the hydrated and dried phases proves impossible based on powder diffraction spectra obtained with conventional high resolution X-ray diffraction equipment.

Chemical Phenomena↗
PubMed2000

[X-ray diffraction Fourier pattern analysis of natural caculus bovis].

OBJECTIVE: To set up a method for analyzing and distinguishing all the chemical components in natural Caoulus Bovis. METHOD: Powder X-ray diffraction analyses was used to analyze four samples of natural Caculus Bovis, and the X-ray diffraction Fourier pattern was obtained for distinguishing natural Caculus Bovis. RESULT AND CONCLUSION: The method can be used for distinguishing animal medicinal materials.

Animals↗
PubMed2001

Detection of low levels of the amorphous phase in crystalline pharmaceutical materials by thermally stimulated current spectrometry.

PURPOSE: To demonstrate the applicability of thermally stimulated current (TSC) spectrometry for the detection of low levels of the amorphous phase in crystalline pharmaceutical materials. METHODS: A crystalline drug substance was melt quenched to produce an amorphous material. Blends of the crystalline and amorphous phases in different ratios (from 75:25 to 99:01) were prepared by serial dilution. TSC studies were performed by applying an electric field at a temperature above the glass transition temperature (Tg) to orient the dipoles, rapidly cooling to 0 degrees C, short circuiting for 1 min, and scanning at 7 degrees C/min to measure the depolarization current. The temperature of the peak in the spectrum corresponds to the Tg of the amorphous phase. Modulated differential scanning calorimtery (DSC) studies were performed using three different test protocols (varying linear heating rate, modulation amplitude, and time period). Powder X-ray diffraction (XRD) studies were performed using a Siemens D500 diffractometer. RESULTS: The ability to detect the amorphous phase by powder XRD is beset with problems due to indirect inference, orientation effects, and instrument-related intensity variations. Even using a consistent sampling procedure and an internal standard, the XRD could quantify the amorphous phase at a level of 5%. In the conventional or modulated DSC, the amorphous phase manifests itself as a shift in the baseline. Using modulated DSC it was possible to detect the amorphous phase at a level of 5% when tested at a heating rate of 2 degrees C/min and an amplitude of +/-1.0 degrees C with a period of 30 s. The moisture sorption method appears to have a similar detection capability. In TSC scans, the glass transition event due to molecular/segmental mobility in the amorphous phase was manifested as a peak/shoulder on the low-temperature side of the depolarization peak of the crystalline phase. The amorphous phase was unambiguously detected at 2% with a lower detection limit of approximately 1%. CONCLUSIONS: On the basis of the results of this preliminary investigation, TSC appears to be capable of detecting the amorphous phase at as low as approximately 1% in crystalline pharmaceuticals, thus offering a much needed capability in discerning factors.

Antihypertensive Agents↗
PubMed2004

Crystal structure and microstructure of some La(2/3-x)Li 3xTiO3 oxides: an example of the complementary use of electron diffraction and microscopy and synchrotron X-ray diffraction to study complex materials.

Three representative oxides of the La(2/3)(-)(x)()Li(3)(x)()TiO(3) system have been studied by selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), and powder synchrotron X-ray diffraction. HRTEM showed that the materials have a complex microstructure. The SAED and HRTEM results have allowed us to propose a model to refine the crystal structure of these oxides that also accounts for their microstructure. The materials have a perovskite-related structure with a diagonal unit cell ( radical 2a(p) x radical 2a(p) x 2a(p)) as a consequence of the tilting of the TiO(6) octahedra. Ordering of lanthanum and lithium ions and vacancies along the 2a(p)-axis, as well as displacements of titanium ions from the center of the octahedra, have been determined. The size and shape of the domains have been obtained from the synchrotron X-ray diffraction data; in addition, other extended defects such as strains and compositional fluctuations have been detected.

Journal Article↗
PubMed2006

Columnar self-assembled ureido crown ethers: an example of ion-channel organization in lipid bilayers.

The self-assembly of ureido crown-ether derivatives has been examined in homogeneous solution, in the solid state, and in planar bilayer membranes. The self-assembly is driven by head-to-tail hydrogen bonding between the urea functional groups. Dimers and higher oligomers are formed in CDCl3 solution as assessed by the change in the ureido NH chemical shift as a function of concentration. Single-crystal X-ray diffraction shows that an antiparallel association of the ureas produces columnar channels composed of face-to-face crown ethers. Powder X-ray diffraction studies also show the presence of a minor phase based upon a parallel urea association leading to an alternative columnar arrangement of the crown ethers. In bilayer membranes at low concentration of ureido crown ether added, membrane disruption is observed together with rare single-channel openings, but at higher concentration, a rich array of interconverting channel conductance states is observed. The channel results are interpreted as arising from discreet stacks of ureido crown ethers where the transport of cations would occur via the macrocycles, admixed with larger pores formed by association of the crown ether headgroups around a central large pore.

Journal Article↗
PubMed1991

An investigation of bioactive glass powders by sol-gel processing.

Bioactive glass powders, with a composition of SiO 2-CaO-P 2O 5, have been successfully synthesized via a sol-gel process at considerably lower temperatures than required for conventional melting methods. Bioactive glass powders made via conventional methods form an interfacial bond with bone when they are implanted. Bonding is correlated with the formation of a surface hydroxyapatite layer. This study examined the formation of a hydroxyapatite layer in Tris-buffered solution as a function of SiO 2 content of sol-gel derived powders. A FT-IRRS technique was used to monitor the formation of the hydroxyapatite on the surface of the powders. X-ray diffraction analysis and BET were also used to characterize the chemical and physical properties of the sol-gel derived bioactive powders. It was discovered that: (a) the rate of hydroxyapatite formation decreased with increasing SiO 2 content for powders whose SiO 2 content was less than 90 mol%; (b) a hydroxyapatite film does not form for the powders whose SiO 2 content is more than 90 mol%; (c) the SiO 2 limit, beyond which the powders lost their bioactivity, was much higher for bioactive glass powders made through sol-gel process (90%) than those made by conventional melting methods (60%). These results indicate that it is possible to significantly expand the bioactive composition range through microstructural control made possible by sol-gel processing techniques.

Glass↗
PubMed2004

Solid-state characterization of rifampicin samples and its biopharmaceutic relevance.

Polymorphism of rifampicin has been postulated to be responsible for its variable bioavailability from solid oral dosage forms. In this regard, it was believed that form II is the preferred form and the content of amorphous needs to be critically monitored. However, there was no study in literature that determines solubility advantage associated with rifampicin polymorphs and further the desired raw material characteristics for the consistent bioavailability. Hence, this investigation was undertaken with an objective to determine biopharmaceutic relevance of rifampicin physical forms and to propose critical raw material specifications for rifampicin bulk material. For this purpose, solid-state properties of standard form I, form II, amorphous and commercial samples acquired from rifampicin manufacturers were characterized by differential scanning calorimetry (DSC), Fourier transformed infrared spectroscopy (FTIR), hot stage microscopy (HSM), thermogravimetric analysis (TGA), powder X-ray diffraction (p-XRD), solid-state nuclear magnetic resonance (NMR) and molecular modelling. In addition, intrinsic dissolution of standard samples, powder dissolution as well as particle size distribution of all the samples and powder dissolution of various sieve fraction of commercial samples were done in order to study the influence of polymorphism and other factors on rate and extent of dissolution. It was found that rifampicin in commercial bulk samples exist as various combinations of form I, form II and amorphous. As physical forms show comparable intrinsic dissolution rate (IDR) at all the pH values, solubility advantage associated with rifampicin polymorphs is negligible. Nevertheless, powder dissolution of commercial samples was influenced by particle size. In powder dissolution of different sieve fractions of commercial samples, fine particles below 100 microm have shown high rate and extent of dissolution irrespective of polymorphic content, whereas particles above 100 microm exhibited reduced dissolution. In intrinsic dissolution, thermodynamically unstable form II exhibited lower IDR than stable form I. Further, this difference is evident only at pH 2.0 and at all other pH values there was no difference in IDR of these two forms. For this unexpected finding, two hypotheses based on differences in H-bonding of the polymorph have been proposed.

Biological Availability↗
PubMed1997

A novel X-ray powder diffractometric method for studying the reaction between pseudoephedrine enantiomers.

The opposite enantiomers of pseudoephedrine were observed to react in the solid state to form the racemic compound. A novel powder X-ray diffractometric method was developed for studying the kinetics and mechanism of this reaction. The powder X-ray diffraction patterns of the enantiomers were identical, but the racemic compound exhibited a different pattern because of its different crystal structure. The powder patterns of the enantiomers and the racemic compound revealed that the 4.62 and 4.25 A lines were unique to the enantiomers and the racemic compound, respectively. Teflon holders were filled with equimolar mixtures of the two enantiomers, and the integrated intensities of the 4.62 and 4.25 A lines were measured at 30-min intervals over a period of 8 h. Thus, the disappearance of the crystalline enantiomers and the appearance of the crystalline racemic compound were quantified simultaneously. The rate of disappearance of the crystalline enantiomers followed a diffusion-controlled reaction model originally proposed by Jander in 1927. During the kinetic experiment, the sum of the weight fractions of the enantiomers and the racemic compound progressively decreased from an initial value of unity suggesting the existence of an intermediate noncrystalline phase. The presence of the noncrystalline phase was confirmed by a steady increase in the background of the X-ray patterns. Thus, the unique ability of the X-ray method to quantify only the crystalline phases has demonstrated the existence of a non-crystalline amorphous intermediate in this solid-solid reaction.

Crystallography, X-Ray↗
PubMed1998

Microfocusing of hard X-rays with cylindrically bent crystal monochromators.

High-energy X-ray focusing with bent-crystal monochromators is known to be hampered by so-called depth or crystal-thickness aberrations. A theoretical model of focus broadening based on the geometrical theory of X-ray diffraction in slightly deformed crystals is presented and compared with experimental data. First, it is shown that depth broadening can be avoided in the Laue geometry by an appropriate choice of asymmetry angle. Based on this finding, a monochromator for high-pressure diffraction experiments has been designed and a source-size-limited focal spot below 10 microns is observed. As a consequence of the box-shaped rocking curve of bent Laue crystals, the focus is free of long-ranging tails. Diffraction patterns of standard powder samples were recorded on imaging plates and a theoretical description of the energy-dispersion-related peak broadening is given. Finally, diffraction patterns of N2 at 180 kbar demonstrate the excellent data quality achievable with this monochromator.

Journal Article↗
PubMed2006

Enhancing the bioavailability of cyclosporine a using solid dispersion containing polyoxyethylene (40) stearate.

Solid dispersion containing polyoxyethylene (40) stearate and cyclosporine A was prepared by solvent-melt method and characterized using differential scanning calorimetry, powder X-ray diffraction, and Infrared Fourier Transform Spectroscopy (FTIR). Dissolution of the drug from solid dispersion was dramatically enhanced compared to that from the drug powder alone and physical mixture. In vivo oral bioavailability of cyclosporine A from the solid dispersion in Wistar rats was comparable to that from a commercial product, Sandimmun Neoral (P>0.05). The formulation is stable up to six months under 30 degrees C/RH60% and one year at 25 degrees C/RH 60% when packed in aluminum-polyethylene laminated bags.

Animals↗
PubMed1997

An investigation of the chemical synthesis and high-temperature sintering behaviour of calcium hydroxyapatite (HA) and tricalcium phosphate (TCP) bioceramics.

The experimental conditions for the synthesis of sub-micrometre, spherical particles of calcium hydroxyapatite [Ca10(PO4)6(OH)2] (HA) and tricalcium phosphate [Ca3(PO4)2] (TCP) are investigated through chemical coprecipitation from the aqueous solutions of calcium nitrate and di-ammonium hydrogen phosphate salts. The precipitation process employed was also found to be suitable for the production of sub-micrometre HA/TCP composite powders in situ. The synthesized pure HA and TCP powders were found to be stable even at 1300 degrees C in air for prolonged heating times. Bioceramic sample characterization was achieved by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and density and surface area measurements. Crystallographic analyses of HA powders were performed by the Rietveld method on the powder XRD data.

Journal Article↗
PubMed2005

Strategies for reducing preferred orientation and strain in powder samples for high-pressure synchrotron X-ray diffraction in diamond-anvil cells.

Among the many problems associated with high-pressure X-ray diffraction from polycrystalline samples in the diamond-anvil cell are strain and preferred orientation. A method is presented for efficiently reducing preferred orientation of powder samples compressed in diamond-anvil cells to pressures in excess of 20 GPa. This method may be successfully applied to samples of yield strength higher than alkalihalides. In addition, the problem of strain is discussed using ice-VII as an example and as an illustration of the importance of laser heating as a method of minimizing strain.

Journal Article↗
PubMed1991

Kinetics of transition of anhydrous carbamazepine to carbamazepine dihydrate in aqueous suspensions.

When suspended in water, anhydrous carbamazepine (C15H12N2O; 1) was transformed to carbamazepine dihydrate (C15H12N2O.2H2O; 2). Compound 1 was dispersed in water at 25 degrees C, and an aliquot of the slurry was taken at periodic intervals and immediately filtered under conditions which removed all the physically bound water from the solid. The weight fractions of 1 and 2 in the solid were quantified by two methods: (a) by determining the weight loss on drying the solid at 60 degrees C under reduced pressure to a constant weight and (b) by a quantitative powder X-ray diffraction technique. There was good agreement between the above two methods. More than 95% (w/w) of 1 was converted to 2 in 1 h and the decrease in the weight fraction of 1 with time was approximately a first-order process.

Carbamazepine↗
PubMed2006

Structure of anhydrous alkali-metal formates.

Single-crystal X-ray diffraction has yielded new crystal structures for cesium formate (CsOOCH) and rubidium formate (RbOOCH). The cesium formate structure has the same unit cell and space group as that published from powder X-ray diffraction data but differs radically in the placement and orientation of the formate ions. The new crystal structure has been successfully modeled with an empirical force field based on pair potentials, whereas it proved impossible to develop a force field that gave an adequate description of the powder structure. For rubidium formate, the gross structure is similar to that previously published, but the space group includes a mirror plane (Pbcm rather than Pbc2(1)). From this information, we have been able to analyze the effect of the cation size on the crystal structure for alkali-metal formates.

Cesium↗
PubMed1989

Polymorphism of sulfathiazole.

The polymorphism of sulfathiazole has been reexamined. The issue of the separate existence of two of the forms, forms III and IV, has now been definitively resolved: both forms exist. Single crystals were used to generate X-ray diffraction patterns, equivalent to those normally obtained from polycrystalline samples, using the ingenious Gandolfi camera. The patterns obtained were distinct and in agreement with the theoretical powder patterns calculated from the reported structures of the two forms, thus confirming the separate existence. Disagreement between the results of previous workers has been traced to two main causes: characterization techniques are not very discriminating for the two forms (III and IV), and the samples examined have invariably been mixtures of III and IV, since the two forms usually crystallize together. Furthermore, crystals of form III exhibit marked preferred orientation, which complicates powder X-ray diffraction (PXRD) analysis. The IR, Raman, and 13C NMR spectra, and PXRD patterns are reported for all four forms. These distinct fingerprints should now enable one to isolate pure samples and to study the properties and the relationships between these forms with full confidence.

Calorimetry, Differential Scanning↗