Development of a new high-performance liquid chromatographic method for the determination of ceftazidime

A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanol-water (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 mu g/mL. The values for interday and intraday precision (relative standard deviation) were < 1 %. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Performance characteristics of bioassay UV-spectrophotometry and high perfomance liquid chromatographic determination of gatifloxacin in tablets

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Performance characteristics of high performance liquid chromatography, first order derivative UV spectrophotometry and bioassay for fluconazole determination in capsules

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Solid-liquid transition in Nb powder determined by third harmonic susceptibility

Measurements of the third harmonic of the AC-susceptibility were employed to determine the boundaries of the linear regime of the magnetic response of Nb powder. Non-linear contributions to the magnetic response reveal the occurrence of a structured phase, disappearing as the vortex lattice melts to the liquid state. A systematic study of the third harmonic was conducted to determine how its onset temperature depends on experimental parameters, such as the frequency and amplitude of the excitation field. The melting line (ML) has been extracted from the onset temperature measured at low-frequencies and low-excitation fields in the presence of DC magnetic fields. The study indicates that the ML can be described by a 3D vortex-glass model, except at lower fields, where the system experiences a depinning crossover, and the best description of the experimental data is provided by a 3D Bose-glass model. (c) 2008 Elsevier B. V. All rights reserved.

Assessment of liquid disposal originated by uranium enrichment at Aramar Experimental Center São Paulo-Brazil

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

High-performance liquid chromatographic separation and identification of polyphenolic compounds from the infusion of Davilla elliptica St. Hill

The isolation of polyphenolic compounds from an infusion of the Brazilian plant Davilla elliptica (Dilleniaceae), used as tea by virtue of its digestive properties, is described. An improved preparative HPLC method was used in order to isolate pure polyphenols from the complex mixture. Liquid-liquid extraction and solid-phase extraction were employed to minimise the interference of polymeric compounds and to provide an enriched fraction of the compounds of interest. The identification of the isolated compounds was performed using analytical HPLC as well as direct injection electrospray ionisation ion trap tandem mass spectrometry (ESI-IT-MS/MS). The high flavonoid content suggests that D. elliptica may be a promising source of compounds to produce natural phytomedicines. Copyright (C) 2007 John Wiley & Sons, Ltd.

Analysis of the accumulated energy by thermal stratification of liquid inside storage tanks with porous layers

A mathematical model was developed in order to study the behavior of thermal stratification of liquid in a typical storage tank with porous medium. The model employs a transient stream function-vorticity formulation to predict the development of stream function and temperature fields in a charging process. Parameters analyzed include Biot, Darcy, Reynolds and Richardson numbers, position, and the thickness of the porous medium. The results show the influence of these physical parameters that should be considered for a good design of storage tanks with thermal stratification.

Occurrence of consonant production errors in liquid phonemes in children with operated cleft lip and palate

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

A liquid phase blocking ELISA for the detection of antibodies against infectious bronchitis virus

A liquid phase blocking ELISA (LPB-ELISA) was developed for the detection and measurement of antibodies against infectious bronchitis virus (IBV). The purified and nonpurified virus used as antigen, the capture and detector antibodies, and the chicken hyperimmune sera were prepared and standardized for this purpose. A total of 156 sera from vaccinated and 100 from specific pathogen-free chickens with no recorded contact with the virus were tested. The respective serum titers obtained in the serum neutralization test (SNT) were compared with those obtained in the LPB-ELISA. There was a high correlation (r2 = 0.8926) between the two tests. The LPB-ELISA represents a single test suitable for the rapid detection of antibodies against bronchitis virus in chicken sera, with good sensitivity (88%), specificity (100%) and agreement (95.31%).

Quantitation of malondialdehyde in gingival crevicular fluid by a high-performance liquid chromatography-based method

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Development and application of methods for determination of residual monomer in dental acrylic resins using high performance liquid chromatography

Two high-performance liquid chromatographic methods for determination of residual monomer in dental acrylic resins are described. Monomers were detected by their UV absorbance at 230 nm, on a Nucleosil((R)) C-18 (5 mu m particle size, 100 angstrom pore size, 15 x 0.46 cm i.d.) column. The separation was performed using acetonitrile-water (55:45 v/v) containing 0.01% triethylamine (TEA) for methyl methacrylate and butyl methacrylate, and acetonitrile-water (60:40 v/v) containing 0.01% TEA for isobutyl methacrylate and 1,6-hexanediol dimethacrylate as mobile phases, at a flow rate of 0.8 mL/min. Good linear relationships were obtained in the concentration range 5.0-80.0 mu g/mL for methyl methacrylate, 10.0-160.0 mu g/mL for butyl methacrylate, 50.0-500.0 mu g/mL for isobutyl methacrylate and 2.5-180.0 mu g/mL for 1,6-hexanediol dimethacrylate. Adequate assay for intra- and inter-day precision and accuracy was observed during the validation process. An extraction procedure to remove residual monomer from the acrylic resins was also established. Residual monomer was obtained from broken specimens of acrylic disks using methanol as extraction solvent for 2 h in an ice-bath. The developed methods and the extraction procedure were applied to dental acrylic resins, tested with or without post-polymerization treatments, and proved to be accurate and precise for the determination of residual monomer content of the materials evaluated. Copyright (c) 2005 John Wiley & Sons, Ltd.

Phenylalanine ammonia-lyase activity in soybean roots extract measured by reverse-phase high performance liquid chromatography

The high performance liquid chromatography (HPLC) technique was applied to measure phenylalanine ammonia-lyase (PAL, EC 4.3.1.5) activity in soybean (Glycine max L. Merril cv. BR16) roots. t-Cinnamate, the catalytic product of the PAL reaction was quantified at 275 nm by isocratic elution with methanol:water through an ODS(M) column. Comparative experiments were carried out with 1.0 mM ferulic acid, an inducer of PAL activity. The results suggest that liquid chromatography is a rapid and sensitive method to analyze PAL activity in non-purified extract.

Evaluation of the biodegradation of different types of lubricant oils in liquid medium

Avaliação da Biodegradação de Diferentes Tipos de Óleo Lubrificante em Meio Aquoso pela Norma Técnica L6.350 (CETESB, 1990), utiliza-se o processo respirométrico de Bartha e Pramer para acompanhar a biodegradação de diferentes tipos de óleo lubrificante automotivo adaptado ao meio aquoso. Para realização do experimento foram preparados um inóculo base e, posteriormente, um inóculo aquoso. Quatro tratamentos foram realizados em dois experimentos consecutivos: T1 (controle); T2 (óleo semi-sintético); T3 (óleo mineral); T4 (óleo usado). Dentre os resultados, obteve-se a seguinte ordem decrescente na produção de CO2 nos respirômetros: T4 > T2 > T3 > T1. Assim, o óleo lubrificante usado surgiu com maior biodegradabilidade, seguido do semisintético e do óleo mineral. Observou-se também que o lubrificante mineral apresentou maior período de adaptação comparado ao semisintético.