Development and validation of a microbiological agar assay for determination of orbifloxacin in pharmaceutical preparations

Orbifloxacin is a fluoroquinolone with broad-spectrum antimicrobial activity, and belongs to the third generation of quinolones. Regarding the quality control of medicines, a validated microbiological assay for determination of orbifloxacin in pharmaceutical formulations has not as yet been reported. For this purpose, this paper reports the development and validation of a simple, sensitive, accurate and reproducible agar diffusion method to quantify orbifloxacin in tablet formulations. The assay is based on the inhibitory effect of orbifloxacin upon the strain of Staphylococcus aureus ATCC 25923 used as test microorganism. The results were treated statistically by analysis of variance and were found to be linear (r = 0.9992) in the selected range of 16.0-64.0 μg/mL, precise with relative standard deviation (RSD) of repeatability intraday = 2.88%, intermediate precision RSD = 3.33%, and accurate (100.31%). The results demonstrated the validity of the proposed bioassay, which allows reliable orbifloxacin quantitation in pharmaceutical samples and therefore can be used as a useful alternative methodology for the routine quality control of this medicine. © 2011 by the authors; licensee MDPI, Basel, Switzerland.

Measurement of angular correlations of jets at s=1.96 TeV and determination of the strong coupling at high momentum transfers

We present a measurement of the average value of a new observable at hadron colliders that is sensitive to QCD dynamics and to the strong coupling constant, while being only weakly sensitive to parton distribution functions. The observable measures the angular correlations of jets and is defined as the number of neighboring jets above a given transverse momentum threshold which accompany a given jet within a given distance δR in the plane of rapidity and azimuthal angle. The ensemble average over all jets in an inclusive jet sample is measured and the results are presented as a function of transverse momentum of the inclusive jets, in different regions of δR and for different transverse momentum requirements for the neighboring jets. The measurement is based on a data set corresponding to an integrated luminosity of 0.7 fb -1 collected with the D0 detector at the Fermilab Tevatron Collider in pp- collisions at s=1.96 TeV. The results are well described by a perturbative QCD calculation in next-to-leading order in the strong coupling constant, corrected for non-perturbative effects. From these results, we extract the strong coupling and test the QCD predictions for its running over a range of momentum transfers of 50-400 GeV. © 2012 Elsevier B.V.

Development and validation of a microbiological assay for determination of chlorhexidine digluconate in aqueous solution

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Electrochemical behavior and voltammetric determination of pyrazinamide using a poly-histidine modified electrode

Pyrazinamide (Pyrazinecarboxamide-PZA) is a drug that is used to treatment tuberculosis. In the present work, the voltammetric behavior of PZA was studied using a screen-printed modified electrode (SPCE). The modified electrode was constructed using poly-histidine films, and it showed an electrocatalytic effect, thus promoting a decrease in PZA reduction potential and improving the voltammetric response. Cyclic voltammetry and electrochemical impedance spectroscopy techniques have been employed in order to elucidate of the electrodic reaction. The results allowed the proposal that in the PZA reduction, a further chemical reaction occurs that corresponds to a second-order process which is subsequent to the electrode reaction. In addition, a sensitive voltammetric method was developed, and it was successfully applied for PZA determination in human urine samples. The best response was found using SPCE modified with poly-histidine prepared by histidine monomer electropolymerization (SPCE/EPH). The electroanalytical performance of the SPCE/EPH was investigated by linear sweep (LSV), differential pulse (DPV), and square wave voltammetry (SWV). A linear relationship between peak current and PZA concentrations was obtained from 9.0 × 10-7 to 1.0 × 10-4 mol L-1 by using DPV. The limit of detection at 5.7 × 10 -7 mol L-1 was estimated, and a relative standard deviation of the 5.0 × 10-6 mol L-1 of PZA of 10 measurement was 3.7%. © 2012 Elsevier B.V. All rights reserved.

GFAAS determination of mercury in muscle samples of fish from Amazon, Brazil

In the present study, a simple, rapid and sensitive method was developed for the determination of mercury concentrations in the muscle tissue of fish from the Brazilian Amazon using graphite furnace atomic absorption spectrometry (GFAAS) following acid mineralization of the samples in an ultrasonic cold water bath. Using copper nitrate as a chemical modifier in solution and sodium tungstate as permanent modifier, we were able to attain thermal stabilization of the mercury up to the atomisation temperature of 1600 °C in the GFAAS assay. The calculated limits of detection (LOD) and quantification (LOQ) were 0.014 and 0.047 mg kg-1, respectively. © 2013 Elsevier Ltd. All rights reserved.

Search for methylation-sensitive amplification polymorphisms in mutant figs

Fig (Ficus carica) breeding programs that use conventional approaches to develop new cultivars are rare, owing to limited genetic variability and the difficulty in obtaining plants via gamete fusion. Cytosine methylation in plants leads to gene repression, thereby affecting transcription without changing the DNA sequence. Previous studies using random amplification of polymorphic DNA and amplified fragment length polymorphism markers revealed no polymorphisms among select fig mutants that originated from gamma-irradiated buds. Therefore, we conducted methylation-sensitive amplified polymorphism analysis to verify the existence of variability due to epigenetic DNA methylation among these mutant selections compared to the main cultivar 'Roxo-de-Valinhos'. Samples of genomic DNA were double-digested with either HpaII (methylation sensitive) or MspI (methylation insensitive) and with EcoRI. Fourteen primer combinations were tested, and on an average, non-methylated CCGG, symmetrically methylated CmCGG, and hemimethylated hmCCGG sites accounted for 87.9, 10.1, and 2.0%, respectively. MSAP analysis was effective in detecting differentially methylated sites in the genomic DNA of fig mutants, and methylation may be responsible for the phenotypic variation between treatments. Further analyses such as polymorphic DNA sequencing are necessary to validate these differences, standardize the regions of methylation, and analyze reads using bioinformatic tools. © FUNPEC-RP.

Determination of Total Nitrosamines in Vegetables Cultivated Organic and Conventional Using Diamond Electrode

Vegetables were analyzed for total N-nitrosamines (NAs) and the influence of disinfection processes was assessed. Differences in NAs found in cabbage, spinach, and broccoli were determined by square wave voltammetry using a boron-doped diamond electrode. Analysis of samples showed that all samples contained detectable levels of NAs but the results indicated that organic contained less than conventionally grown products. The sum of the total NAs was higher in the cabbage samples, ranging between 2.8-3.1 ppb and lower in broccoli samples at 0.2-1.1 ppb. The method described is simple, rapid, selective, and sensitive. The results suggested that the disinfection process affects the level of NAs, in this manner affecting the level of human exposure to NAs. © 2012 Springer Science+Business Media New York.

Electrochemical sensor for ranitidine determination based on carbon paste electrode modified with oxovanadium (IV) salen complex

The preparation and electrochemical characterization of a carbon paste electrode modified with the N,N-ethylene-bis(salicyllideneiminato)oxovanadium (IV) complex ([VO(salen)]) as well as its application for ranitidine determination are described. The electrochemical behavior of the modified electrode for the electroreduction of ranitidine was investigated using cyclic voltammetry, and analytical curves were obtained for ranitidine using linear sweep voltammetry (LSV) under optimized conditions. The best voltammetric response was obtained for an electrode composition of 20% (m/m) [VO(salen)] in the paste, 0.10 mol L- 1 of KCl solution (pH 5.5 adjusted with HCl) as supporting electrolyte and scan rate of 25 mV s- 1. A sensitive linear voltammetric response for ranitidine was obtained in the concentration range from 9.9 × 10- 5 to 1.0 × 10- 3 mol L- 1, with a detection limit of 6.6 × 10- 5 mol L- 1 using linear sweep voltammetry. These results demonstrated the viability of this modified electrode as a sensor for determination, quality control and routine analysis of ranitidine in pharmaceutical formulations. © 2013 Published by Elsevier B.V.

Cross linked Poly (4-Vinylpyridine-Ethylene Glycol Dimethacrylate) Used for Preconcentration of Cd(II) and its Determination by Flow Injection Flame Atomic Absorption Spectrometry

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Screening and determination of sulphonamide residues in bovine milk samples using a flow injection system

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Sensitive flow-injection spectrophotometric analysis of bromopride

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Simultaneous determination of epinephrine and dopamine by electrochemical reduction on the hybrid material SiO2/graphene oxide decorated with Ag nanoparticles

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

Development of biomimetic sensor for fast and sensitive detection of Norfloxacin

A biomimetic sensor is proposed as a promising new analytical method for determination of norfloxacin (NF) in pharmaceuticals. The sensor was prepared by modifying a glassy carbon electrode surface with a Nafion® membrane doped with poly(copper phthalocyanine) complex [poly-CuPc]. Amperometric measurements carried out with the sensor under an applied potential of -0.05 V vs Ag|AgCl in 0.1 mol L-1 acetic acid containing 1.5 × 10-3 mol L-1 hydrogen peroxide showed a linear response range from 2.0 × 10-4 to 1.2 × 10-3 mol L-1. Selectivity and interference studies were also performed. A sensor response mechanism is proposed, based on the experimental evidence. Recovery studies were carried out using environmental samples, in order to evaluate the sensor’s potential for use with these sample classes. Finally, sensor performance was evaluated using analyses of commercial formulations.

Determination of anticonvulsants in human plasma using SPME in a heated interface coupled online to liquid chromatography (SPME-LC)

A simple and sensitive method using solid phase microextraction (SPME) and liquid chromatography (LC) with heated online desorption (SPME-LC) was developed and validated to analyze anticonvulsants (AEDs) in human plasma samples. A heated lab-made interface chamber was used in the desorption procedure, which allowed the transference of the whole extracted sample. The SPME conditions were optimized by applying an experimental design. Important factors are discussed such as fiber coating types, pH, extraction time and desorption conditions. The drugs were analyzed by LC, using a C18 column (150 mm 4.6 mm 5 mm); and 50 mmol L1 , pH ¼ 5.50 ammonium acetate buffer : acetonitrile : methanol (55 : 22 : 23 v/v) as the mobile phase with a flow rate of 0.8 mL min1 . The suggested method presented precision (intra-assay and inter-assay), linearity and limit of quantification (LOQ) all adequate for the therapeutic drug monitoring (TDM) of AEDs in plasma.

Development of a simple method for determination of NO2 in air using digital scanner images

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)