Quantitative thin-layer chromatographic method of analysis of azithromycin in pure and capsule forms

A validated stability-indicating thin-layer chromatographic (TLC) method of the analysis of azithromycin (AZT) in bulk and capsule forms is developed. Both AZT potential impurity and degradation products can be selectively and accurately estimated in both raw material and product onto one precoated silica-gel TLC plate 60F254. The development system used is n-hexane-ethyl acetate-diethylamine (75:25:10, v/v/v). The separated bands are detected as brown to brownish red spots after spraying with modified Dragendorff's solution. The Rf values of AZT, azaerythromycin A, and the three degradation products are 0.54, 0.35, 0.40, 0.20, and 0.12, respectively. The optical densities of the separated spots are found to be linear in proportion to the amount used. The stress testing of AZT shows that azaerythromycin A is the major impurity and degradation product, accompanied by three other unknown degradation products. The stability of AZT is studied under accelerated conditions in order to provide a rapid indication of differences that might result from a change in the manufacturing process or source of the sample. The forced degradation conditions include the effect of heat, moisture, light, acid-base hydrolysis, sonication, and oxidation. The compatibility of AZT with the excipients used is also studied in the presence and absence of moisture. The amounts of AZT and azaerythromycin A are calculated from the corresponding linear calibration curve; however, the amounts of any other generated or detected unknown impurities are calculated as if it were AZT. This method shows enough selectivity, sensitivity, accuracy, precision, linearity-range, and robustness to satisfy Federal Drug Administration/International Conference of Harmonization regulatory requirements. The method developed can also be used for the purity testing of AZT raw material and capsules, content uniformity testing, dissolution testing, and stability testing of AZT capsules. The potential impurity profiles of both active AZT material and capsule forms are found comparable. The linear range of AZT is between 5 and 30 mcg/spot with a limit of quantitation of 2 mcg/spot. The intraassay relative standard deviation percentage is not more than 0.54%, and the day-to-day variation is not more than 0.86%, calculated on the amounts of AZT RS recovered using different TLC plates.     

Pyrazolones and quinoxalines from 4-phenyl-2,3-dioxobutyro-1,4-lactone

4-Phenyl-2,3-dioxobutyro-1,4-lactone ( 1 ) gave with phenylhydrazine and ils p-Cl, p-Br, p-I and p-NO₂ derivatives, bishydrazones which were eyclized to 1-aryl-3-(α-hydroxybenzyl)-4,5-dione-4-arylhydrazones. With o-phenylene diamine, compound 1 gave either a Schiff base or a substituted quinoxaline, depending upon the ratio of the reactants.     

Heteronuclear 3 d/DyIII Coordination Clusters as Catalysts in a Domino Reaction

Three isoskeletal tetranuclear coordination clusters with general formula [M^II₂Dy^III₂L₄(EtOH)₆](ClO₄)₂?2 EtOH, (M=Co, 1 ; M=Ni, 2 ) and [Ni^II₂Dy^III₂L₄Cl₂(CH₃CN)₂]?2 CH₃CN ( 3 ), have been synthesized and characterized. These air‐stable compounds, and in particular 3 , display efficient homogeneous catalytic behavior in the room‐temperature synthesis of trans‐4,5‐diaminocyclopent‐2‐enones from 2‐furaldehyde and primary or secondary amines under a non‐inert atmosphere.     

Local and global existence of solutions for a class of integro-differential equations with delay

In this article we consider a class of first order nonlinear integro-differential equations with delay. We propose new approach for investigating local and global existence of the solutions of its Cauchy problem. This approach gives new results.     

Synthesis of norbornenes containing cationic mono‐ and di(cyclopentadienyliron)arene complexes and their ring‐opening metathesis polymerization

A number of classes of polynorbornenes containing cationic iron moieties within their side chains were prepared via ring‐opening metathesis polymerization with a ruthenium‐based catalyst. The iron‐containing polymers displayed excellent solubility in polar organic solvents. The weight‐average molecular weights of these polymeric materials were estimated to be in the range of 18,000–48,000. Thermogravimetric analysis of these polymers showed two distinct weight losses. The first weight loss was in the range of 204–260 °C and was due to the loss of the metallic moieties, whereas the second weight loss was observed at 368–512 °C and was due to the degradation of the polymer backbone. Cyclic voltammetry studies of the iron‐containing polymers showed that the 18 e^? cationic iron centers underwent a reduction to give the neutral 19 e^? complexes at half‐wave potential (E_1/2) = ?1.105 V. Photolysis of the metallated polymers led to the isolation of the norbornene polymers in very good yields. Differential scanning calorimetry studies showed a sharp increase in the glass‐transition temperatures up to 91 °C when rigid aromatic side chains were incorporated into the norbornene polymers. © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 3053–3070, 2006     

Chemical Reaction Effect on Convection in Bidispersive Porous Medium

Transport in Porous Media - The object of this study is to investigate the question of convective movement of a reacting solute in a viscous incompressible occupying a plane layer in a saturated...     

A New Fourier Truncated Regularization Method for Semilinear Backward Parabolic Problems

We study the backward problem for non-linear (semilinear) parabolic partial differential equations in Hilbert spaces. The problem is severely ill-posed in the sense of Hadamard. Under a weak a priori assumption on the exact solution, we propose a new Fourier truncated regularization method for stabilising the ill-posed problem. In comparison with previous studies on solving the nonlinear backward problem, our method shows a significant improvement.     

Effect of the preparation route on the structure and microstructure of LaCoO3

Lanthanum cobaltite oxide, LaCoO₃, was prepared by the evaporation technique and the amorphous metal complex method. Powders were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and surface area measurements. The effect of the synthesis route on the phase purity, particle size, surface area, and morphology of the powders was studied. A single perovskite phase was synthesized at 700°C using the amorphous metal complex route. However, the evaporation technique required higher temperature for LaCoO₃ crystallization. Based on the characterization results, low temperature formation of LaCoO₃ was attributed to the homogeneity of the precursors. Such behavior also results in different microstructures. Powder synthesized by the amorphous metal complex method exhibited the highest surface area and the lowest particle size.