A robust multi‐grid pressure‐based algorithm for multi‐fluid flow at all speeds

This paper reports on the implementation and testing, within a full non‐linear multi‐grid environment, of a new pressure‐based algorithm for the prediction of multi‐fluid flow at all speeds. The algorithm is part of the mass conservation‐based algorithms (MCBA) group in which the pressure correction equation is derived from overall mass conservation. The performance of the new method is assessed by solving a series of two‐dimensional two‐fluid flow test problems varying from turbulent low Mach number to supersonic flows, and from very low to high fluid density ratios. Solutions are generated for several grid sizes using the single grid (SG), the prolongation grid (PG), and the full non‐linear multi‐grid (FMG) methods. The main outcomes of this study are: (i) a clear demonstration of the ability of the FMG method to tackle the added non‐linearity of multi‐fluid flows, which is manifested through the performance jump observed when using the non‐linear multi‐grid approach as compared to the SG and PG methods; (ii) the extension of the FMG method to predict turbulent multi‐fluid flows at all speeds. The convergence history plots and CPU‐times presented indicate that the FMG method is far more efficient than the PG method and accelerates the convergence rate over the SG method, for the problems solved and the grids used, by a factor reaching a value as high as 15. Copyright © 2003 John Wiley & Sons, Ltd.     

A numerical method for solving the Fredholm integral equation of the second kind

The numerical method is used to solve the Fredholm integral equation of the second kind with weak singular kernels using the Toeplitz matrices. The solution has a computing time requirement ofO(N ²), where 2N + 1 is the number of discretization points used. Also, the error estimate is computed. Some numerical examples are computed using the MathCad package.     

A selective spectrophotometric method for determination of rosoxacin antibiotic using sodium nitroprusside as a chromogenic reagent

A selective spectrophotometric method for the determination of rosoxacin (ROS), a 4-quinolone antimicrobial agent, has been developed and validated. The method was based on the reaction of ROS with alkaline sodium nitroprusside (SNP) reagent at room temperature forming a red colored chromogen measured at 455 nm. The conditions affecting the reaction (SNP concentration, pH, color-developing time, temperature, diluting solvent and chromogen stability time) were optimized. Under the optimum conditions, good linear relationship (r=0.9987) was obtained between the absorbance and the concentration of ROS in the range of 20-50 microg ml(-1). The assay limits of detection and quantitation were 2.5 and 8.4 microg ml(-1), respectively. The method was successfully applied to the analysis of bulk drug and laboratory-prepared tablets; the mean percentage recoveries were 100.1+/-0.33 and 101.24+/-1.28%, respectively. The results were compared favourably with those obtained by the reported method; no significant difference in the accuracy and precision as revealed by the accepted values of t- and F-tests, respectively. The robustness and ruggedness of the method was checked and satisfactory results were obtained. The proposed method was found to be highly selective for ROS among the fluoroquinolone antibiotics. The reaction mechanism was proposed and it proceeded in two steps; the formation of nitroferrocyanide by the action of sodium hydroxide alkalinity on SNP and the subsequent formation of the colored nitrosyl-ROS derivative by the attack at position 6 of ROS.     

The use of phosphine ligands to control the regiochemistry of Pd-catalyzed hydrostannations of 1-alkynes: synthesis of (E)-1-tributylstannyl-1-alkenes

The regiochemistry of palladium-catalyzed hydrostannations of terminal alkynes is dramatically influenced by ligand effects. Use of phosphines such as Cy3P, t-Bu2PCH2t-Bu, and t-Bu3P provides (E)-1-tributylstannyl-1-alkenes with regioselectivities up to >99:<1 for substrates where the commonly used Ph3P shows much lower regioselectivities.     

Simultaneous multiresidue determination of tetracyclines and fluoroquinolones in catfish muscle using high performance liquid chromatography with fluorescence detection

Efficient methods are needed for analysis of veterinary drug residues in food. A number of methods are available for single analytes. Multiresidue methods are now increasingly available. It is still rare, however, to find methods not involving mass spectrometry which allow for analysis of more than one class of drug residue. An efficient multiresidue method for the simultaneous determination of fluoroquinolones (FQs) and tetracyclines (TCs) in catfish muscle has now been developed. This method involves an extraction of the analytes with a mixture of acetonitrile and citrate buffer containing magnesium chloride. After centrifugation and evaporation of the supernatants, the residues are determined using high performance liquid chromatography with fluorescence detection. With this method, five fluoroquinolones and three tetracyclines were determined in fortified catfish muscle at levels of 20, 50, and 100 ng g(-1). Average recoveries for ciprofloxacin (CIP), sarafloxacin (SAR), danofloxacin (DANO), enrofloxacin (ENRO), difloxacin (DIF), oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) were in the range of 60-92% with good relative standard deviations. The limits of quantitation ranged from 0.15 to 1.5 ng g(-1). Utilization of the method to successfully analyze catfish muscle samples incurred with enrofloxacin and with oxytetracycline is described.     

LC–MS/MS method for the quantification of masitinib in RLMs matrix and rat urine: application to metabolic stability and excretion rate

Masitinib (MST) is a selective tyrosine kinase inhibitor. Validated liquid chromatography tandem mass spectrometric method (LC–MS/MS) was developed for the quantification of MST in rat liver microsomes (RLMs) matrix. The developed method was applied to metabolic stability and excretion rate studies. Reversed phase liquid chromatography was used for resolution of MST and bosutinib (IS) using C₁₈ (50 mm × 2.1 mm, 1.8 μm). Binary solvent system consisted of 35% solvent A (0.1% formic acid in H₂O, pH: 3.2) and 65% solvent B (acetonitrile) used as mobile phase at flow rate of 0.25 mL with a total run time of 5 min. Injection volume was 5 µL. Generation of ions was done in positive ESI source and quantification of MST and IS were done using MRM mode. The developed method showed a linearity in the range of 5–200 ng/mL (r² ≥ 0.9992) with LOQ and LOD of 0.25 and 0.76 ng/mL in RLMs. The intra- and inter-day precision and accuracy ranged from 0.95 to 1.49 and ? 5.22 to 1.13%, respectively in RLMs. Rate of disappearance of MST during incubation with RLMs was almost linear allover incubation time. In vitro t_1/2 was 50.38 min and CL_in was 3.11 ± 0.2. The developed method was applied also to measure the rate of masitinib excretion in rat urine. The method can used for further pharmacokinetic studies of MST.     

Efficient synthesis of CN2097 using in situ activation of sulfhydryl group

CN2097 (R₇Cs-sCYK[KTE(β-Ala)]V) is a rationally designed peptidomimetic that shows effectiveness in preclinical models for the treatment of neurological disorders, such as Angelman syndrome, traumatic brain injury (TBI), and stroke. Because of its potential therapeutic activity for the treatment of human CNS disorders, there was an urgent need to develop an efficient strategy for large-scale synthesis of CN2097. The synthesis of CN2097 was accomplished using Fmoc/tBu solid phase chemistry in multiple steps. Two different peptide fragments (activated polyarginine peptide Npys-sCR₇ and CYK[KTE(β-Ala)]V) were synthesized, followed by solution phase coupling in water. Activation of the polyarginine (CR₇) was achieved in situ during cleavage of protected peptide (C(Trt)R(Pbf)₇) from the Rink amide resin using 5 equiv. of 2,2-dithopyridine in TFA:TIS:H₂O (95:2.5:2.5, v/v/v) for 4 h. The disulfide coupling was efficient which provided a 60% yield.     

Development of Two Innovative 96-Microwell-Based Spectrophotometric Assays with High Throughput for Determination of Fluoroquinolone Antibiotics in their Pharmaceutical Formulations

Journal of Applied Spectroscopy - Fluoroquinolone antibiotics (FQAs) have broad-spectrum antibacterial activity, high potency, variable indications, and excellent pharmacokinetic profi les. Many...     

Development of a novel 96-microwell assay with high throughput for determination of olmesartan medoxomil in its tablets

A novel 96-microwell-based spectrophotometric assay has been developed and validated for determination of olmesartan medoxomil (OLM) in tablets. The formation of a colored charge-transfer (CT) complex between OLM as a n-electron donor and 2, 5-dichloro-3, 6-dihydroxy-1, 4-benzoquinone (p-chloranilic acid, pCA) as a π-electron acceptor was investigated, for the first time, and employed as a basis in the development of the proposed assay. The proposed assay was carried out in 96-microwell plates. The absorbance of the colored-CT complex was measured at 490 nm by microwell-plate absorbance reader. The optimum conditions of the reaction and the analytical procedures of the assay were established. Under the optimum conditions, linear relationship with good correlation coefficient was found between the absorbance and the concentration of OLM in the range of 1-200 μg ml^-1. The limits of detection and quantitation were 0.3 and 1 μg ml^-1, respectively. No interference was observed from the additives that are present in the pharmaceutical formulation or from hydrochlorothiazide and amlodipine that are co-formulated with OLM in some formulations. The assay was successfully applied to the analysis of OLM in tablets with good accuracy and precision. The assay described herein has great practical value in the routine analysis of OLM in quality control laboratories, as it has high throughput property, consumes minimum volume of organic solvent thus it offers the reduction in the exposures of the analysts to the toxic effects of organic solvents, and reduction in the analysis cost by 50-fold. Although the proposed assay was validated for OLM, however, the same methodology could be used for any electron-donating analyte for which a CT reaction can be performed.     

Optical properties of nanostructured InSe thin films

Thin films of InSe were prepared by thermal evaporation technique. The as-deposited films have nano-scale crystalline nature and the annealing enhanced the degree of crystallinity. The optical properties of nanocrystalline thin films of InSe were studied using spectrophotometric measurements of transmittance, T, and reflectance, R, at normal incidence of light in the wavelength range 200–2500 nm. The optical constants (refractive index, n, and absorption index, k) were calculated using a computer program based on Murmann's exact equations. The calculated optical constants are independent of the film thickness. The optical dispersion parameters have been analysed by single oscillator model. The type of transition in InSe films is indirect allowed with a value of energy gap equals to 1.10 eV, which increased to 1.23 eV upon annealing.