Comparison of the quantification of caffeine in human plasma by gas chromatography and ELISA

In the present study we evaluated the precision of the ELISA method to quantify caffeine in human plasma and compared the results with those obtained by gas chromatography. A total of 58 samples were analyzed by gas chromatography using a nitrogen-phosphorus detector and routine techniques. For the ELISA test, the samples were diluted to obtain a concentration corresponding to 50% of the absorbance of the standard curve. To determine whether the proximity between the I50 of the standard curve and that of the sample would bring about a more precise result, the samples were divided into three blocks according to the criterion of difference, in modulus, of the I50 of the standard curve and of the I50 of the sample. The samples were classified into three groups. The first was composed of 20 samples with I50 up to 1.5 ng/ml, the second consisted of 21 samples with I50 ranging from 1.51 to 3 ng/ml, and the third of 17 samples with I50 ranging from 3.01 to 13 ng/ml. The determination coefficient (R² = 0.999) showed that the data obtained by gas chromatography represented a reliable basis. The results obtained by ELISA were also reliable, with an estimated Pearson correlation coefficient of 0.82 between the two methods. This coefficient for the different groups (0.88, 0.79 and 0.49 for groups 1, 2 and 3, respectively) showed greater reliability for the test with dilutions closer to I50.

Feed digestibility and productive performance of bullfrogs fed in high and low frequency

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

Multi-spectroscopic monitoring of cisplatin-derived species delivery from ureasil polyether hybrid matrix

Driven by the challenges involved in the development of new advanced materials with unusual drug delivery profiles capable of improving the therapeutic and toxicological properties of existing cancer chemotherapy, the one-pot sol-gel synthesis of flexible, transparent and insoluble urea-cross-linked polyether-siloxane hybrids has been recently developed. In this one-pot synthesis, the strong interaction between the antitumor cisplatin (CisPt) molecules and the ureasil-poly(propylene oxide) (PPO) hybrid matrix gives rise to the incorporation and release of an unknown CisPt-derived species, hindering the quantitative determination of the drug release pattern from the conventional UV-Vis absorption technique. In this article, we report the use of an original synchrotron radiation calibration method based on the combination of XAS and UV-Vis for the quantitative determination of the amount of Pt-based molecules released in water. Thanks to the combination of UV-Vis, XAS and Raman techniques, we demonstrated that both the CisPt molecules and the CisPt-derived species are loaded into an ureasil-PPO/ureasil-poly(ethylene oxide) (PEO) hybrid blend matrix. The experimentally determined molar extinction coefficient of the CisPt-derived species loaded into ureasil-PPO hybrid matrix enabled the simultaneous time-resolved monitoring of each Pt species released from this hybrid blend matrix.

An environmentally friendly reflectometric method for ranitidine determination in pharmaceuticals and human urine

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

An Environmentally Friendly Reflectometric Method for Bumetanide Determination in Pharmaceuticals

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

Cathodic stripping voltammetric determination of cefaclor in pharmaceutical formulations

A sensitive method is described for the determination of cefaclor by cathodic stripping voltammetry at the hanging mercury drop electrode. cefaclor is accumulated at the electrode surface as a mercury salt, which is reduced at -0.67 V. The optimum accumulation potential and accumulation time were +0.15 V and up to 180 s, respectively. Linear calibration graphs were obtained between 3.9 mu g.L-1 to 39 mu g.L-1 and the limit of determination was evaluated to be 1.9 mu g.L-1. The method was applied successfully to the determination of cefaclor in pharmaceutical formulations.

Flow injection amperometric detection of ascorbic acid using a Prussian Blue film-modified electrode

The PB film-modified electrode was used as an amperometric detector for flow injection analysis of ascorbic acid. The modified electrode detector showed good sensitivity, stability and reproducibility. The calibration curve for ascorbic acid was linear over the concentration range from 5.0 x 10(-6) to 1.0 x 10(-3) mol l(-1) with a slope of 19.9 mA mol(-1) per litre and a correlation coefficient of 0.999. The detection limit of this method was 2.49 x 10(-6) mol l(-1). The relative standard deviation of six replicate injections of 2.5 x 10(-4) mol l(-1) ascorbic acid was 2.5%. The results obtained for ascorbic acid determination in pharmaceutical products are in good agreement with those obtained by using the procedure involving the reaction between triiodide and ascorbic acid. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Determination of buprofezin, pyridaben, and tebufenpyrad residues by gas chromatography mass-selective detection in clementine citrus

A gas chromatography-mass-selective (GC-MS) detection method to determine buprofezin, pyridaben, and tebufenpyrad on the pulp, peel, and whole fruit of clementines is described. The extraction/partition procedure was performed in one step and no cleanup was necessary with the GC-MS in the SIM-mode pesticide determination. Recovery ranged from 75 to 124% with coefficients of variance ranging between 1 and 13%. The limit of determination was 0.01 mg/kg for all pesticides. The field trials showed a similar degradative behavior for all active ingredients (AI), with a great residue decrease during the first week and stability in the second. Just after treatment buprofezin and tebufenpyrad showed lower residues than the maximum residue limit (MRL) fixed in Italy, while pyridaben was below the MRL after a week.

Determination and persistence of methiocarb in artichokes

A simple and rapid method for the determination of methiocarb in artichokes by high-performance liquid chromatography with UV detection is described. No derivatization is needed and the limit of determination (0.01 ppm) is analogous to that of fluorometric detection. The results of trials carried out with granular and liquid formulations of this active ingredient are also reported. Immediately after treatment with the liquid formulation methiocarb residues averaged 1.47 ppm, while after treatment with the granular formulation residues were considered fortuitous. The decay rate of methiocarb residues in artichokes shows that the decrease and eventual disappearance of this active ingredient can chiefly be ascribed to the dilution effect due to head growth.

Gas Chromatographic Determination of Cyprodinil, Fludioxonil, Pyrimethanil, and Tebuconazole in Grapes, Must, and Wine

A rapid and simple gas chromatographic method for determinating cyprodinil, fludioxonil, pyrimethanil, and tebuconazole in grapes, must, and wine is described. An on-line microextraction method was used with a one-step extraction-partition procedure. Nitrogen-phosphorus and mass spectrometric detectors were used, because of their low sensitivity and high selectivity. Because of high selectivity of detector, no cleanup was necessary and the extract was concentrated 5 times. Recoveries from fortified grapes, must, and wine ranged from 93 to 110%. Limits of determination were 0.05 mg/kg for cyprodinil and pyrimethanil and 0.10 mg/kg for fludioxonil and tebuconazole.

A multicommuted flow-based system for hydrogen peroxide determination by chemiluminescence detection using a photodiode

A simple, rapid, and automated assay for hydrogen peroxide in pharmaceutical samples was developed by combining the multicommutation system with a chemiluminescence (CL) detector. The detection was performed using a spiral flow-cell reactor made from polyethylene tubing that was positioned in front of a photodiode. It allows the rapid mixing of CL reagent and analyte and simultaneous detection of the emitted light. The chemiluminescence was based on the reaction of luminol with hydrogen peroxide catalyzed by hexacyanoferrate(III). The feasibility of the flow system was ascertained by analyzing a set of pharmaceutical samples. A linear response within the range of 2.2-210 μmol l-1 H2O2 with a LD of 1.8 μmol l-1 H2O2 and coefficient of variations smaller than 0.8% for 1.0×10-5 mol l-1 and 6.8×10-5 mol l-1 hydrogen peroxide solutions (n=10) were obtained. Reagents consumption of 90 μg of luminol and 0.7 mg of hexacyanoferrate(III) per determination and sampling rate of 200 samples per hour were also achieved. Copyright © Taylor & Francis Group, LLC.

Validation of an alternative analytical method for the quantification of antioxidant activity in plant extracts

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Carbon paste electrode modified with ascorbic acid and carbon nanotubes for determination copper in sugar cane spirit

This work has been carried out in order to determine the copper content in sugar cane spirit samples from the south of Minas Gerais, using a carbon paste electrode modified with ascorbic acid and carbon nanotubes using the square wave voltammetry technique. The following parameters were studied: Ed (deposit potencial). Td (deposit time), f (frequency), A (amplitude) and ΔEs (increment scanning). The analytical curve was built in an interval from 0.5 to 12 mg L-1 and a coefficient of linear correlation of 0.997 Three sugar cane spirit samples were analysed, which presented copper content ranging from 0.29 to 1.59 mg L-1.

Evaluation via multivariate techniques of scale factor variability in the rietveld method applied to quantitative phase analysis with X ray powder diffraction

ABSTRACT: The present work uses multivariate statistical analysis as a form of establishing the main sources of error in the Quantitative Phase Analysis (QPA) using the Rietveld method. The quantitative determination of crystalline phases using x ray powder diffraction is a complex measurement process whose results are influenced by several factors. Ternary mixtures of Al2O3, MgO and NiO were prepared under controlled conditions and the diffractions were obtained using the Bragg-Brentano geometric arrangement. It was possible to establish four sources of critical variations: the experimental absorption and the scale factor of NiO, which is the phase with the greatest linear absorption coefficient of the ternary mixture; the instrumental characteristics represented by mechanical errors of the goniometer and sample displacement; the other two phases (Al2O3 and MgO); and the temperature and relative humidity of the air in the laboratory. The error sources excessively impair the QPA with the Rietveld method. Therefore it becomes necessary to control them during the measurement procedure.

Procedures to Evaluate the Efficiency of Protective Clothing Worn by Operators Applying Pesticide

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