Characterization and quantitation of clarithromycin polymorphs by powder X-ray diffractometry and solid-state NMR spectroscopy.
Characterization of clarithromycin polymorph was performed by solid-state cross polarization and magic angle spinning (CP/MAS) 13C-NMR spectroscopy. Two polymorphs, form II and form I, of clarithromycins indicated characteristic resonances of C1 carbonyl carbon at 176.2 and 175.2 ppm, respectively. Since each peak of C1 carbon was well separated in the spectrum of the two polymorphs, we performed quantitative analysis of the polymorphic fraction from the peak area of these peaks. The peak area of form I was found to linearly increase with an increase of its content, with a correlation coefficient of above 0.99. Solid-state NMR was found to be a useful technique to determine the characteristics of the polymorphic forms. (+info)
X-ray powder diffraction patterns for certain beta-lactam, tetracycline and macrolide antibiotic drugs.
X-ray powder diffraction (XRD) data for eight beta-lactam viz., ampicillin sodium, ampicillin trihydrate, penicillin G procaine, benzathine penicillin, benzyl penicillin sodium, cefalexin, cefotaxime sodium and ceftriaxone sodium; three tetracyclines viz., doxycycline hydrochloride, oxytetracycline dihydrate and tetracycline hydrochloride; and two macrolide viz., azithromycin and erythromycin estolate antibiotic drugs were obtained using a powder diffractometer. The drugs were scanned from Bragg angles (2theta) of 10 degrees to 70 degrees. The obtained data were tabulated in terms of the lattice spacing (A) and relative line intensities (I/I(I)). This new information may be useful for identifying these drugs from confiscated materials, which has been frequently encountered in forensic laboratories. (+info)
Crystal lattice as biological phenotype for insect viruses.
Many insect viruses survive for long periods by occlusion within robust crystalline polyhedra composed primarily of a single polyhedrin protein. We show that two different virus families form polyhedra which, despite lack of sequence similarity in the virally encoded polyhedrin protein, have identical cell constants and a body-centered cubic lattice. It is almost inconceivable that this could have arisen by chance, suggesting that the crystal lattice has been preserved because it is particularly well-suited to its function of packaging and protecting viruses. (+info)
Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry.
Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system. (+info)
Specific inclusion mode of guest compounds in the amylose complex analyzed by solid state NMR spectroscopy.
The inclusion compound formation between linear amylose of molecular weight 102500 (AS100) and p-aminobenzoic acid (PA) during the sealed-heating process was investigated by powder X-ray diffractometry, infrared spectroscopy and solid state NMR spectroscopy. Sealed-heating of AS100 and PA at 100 degrees C for 6 h provided an inclusion compound with 6(1)-helix structure, while a 7(1)-helix structure was found when sealed-heating was carried out at 150 degrees C for 1 h. The formation of an inclusion compound was not observed when sealed-heating was performed at 50 degrees C for 6 h. The 7(1)-helix inclusion compound maintained its structure even during storage at high temperature while the 6(1)-helix inclusion compound decomposed and returned to the original V(a)-amylose upon heating to 180 degrees C. Quantitative determination revealed that one PA molecule could be included per one helical turn of AS100 for both 6(1)-helix and 7(1)-helix inclusion compounds. Solid state NMR spectroscopy suggested that PA molecules were included in the amylose helix core in the 7(1)-helix inclusion compound, while in the case of 6(1)-helix inclusion compound, PA molecules were accommodated in the interstices between amylose helices. Moreover, the inclusion compound formation by sealed-heating of AS100 was also observed when using PA analogues as guest compounds. The binding ratio of AS100 and PA analogues varied depending on the size of guest molecules. (+info)
Preparation, characterization and in vitro dissolution studies of solid systems of valdecoxib with chitosan.
In the present study, the solubilizing and amorphizing properties of Valdecoxib (a poorly water soluble anti inflammatory drug) with low molecular weight chitosan (a polymer), have been investigated. Binary systems of varying drug/polymer ratios were prepared using different techniques (physical mixing, co-grinding, kneading) and were tested for dissolution. Drug carrier interactions were investigated in both the liquid and solid state, by phase solubility analysis, differential scanning calorimetry, powder X-ray diffractrometry, FT-IR spectroscopy and scanning electron microscopy. The solubility of the drug increased with increasing polymer concentration showing A(N) type phase solubility diagram. Differential scanning calorimetry, powder X-ray diffractrometry and scanning electron microscopic studies of binary systems suggested generation of amorphous form of drug (in kneading and co ground mixtures). IR spectroscopy revealed the presence of hydrogen bonding in kneading and co ground mixtures. Drug dissolution was improved with increasing the polymer concentration in the mixture (Kneaded>co ground>physical mixture), which was attributed to the amorphonization and/or decreased drug crystallinity, size and polymer wetting effect. Enhanced dissolution combined with its direct compression feasibility and anti ulcerogenic action results in low molecular weight chitosan for developing fast release oral solid dosage forms of valdecoxib. (+info)
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. (+info)
Development of prednisone:polyethylene glycol 6000 fast-release tablets from solid dispersions: solid-state characterization, dissolution behavior, and formulation parameters.