Biomedical subjects

M C Sampedro

Publications and source records attributed to M C Sampedro.

7 recordsLinked to original sources

PubMed2005

Solid-phase microextraction coupled with high performance liquid chromatography using on-line diode-array and electrochemical detection for the determination of fenitrothion and its main metabolites in environmental water samples.

The aim of this study was to develop a methodology for the analysis of the insecticide fenitrothion and its two main environmental metabolites, fenitrooxon and 3-methyl-4-nitrophenol. For this purpose, a solid-phase microextraction (SPME) method coupled to high performance liquid chromatography (LC) was optimized. Two on-line detectors, diode array (DAD) and direct current amperometrical (DCAD) were used in order to determine sensitivity and selectivity. The effects of the extraction parameters, including exposure and desorption time, pH, temperature, salt concentration and desorption mode on the extraction efficiency were studied. A satisfactory reproducibility for extractions from samples at 20 ppb-level with RSD < 12.5% (n = 10) was obtained. The calibration graphs were linear in the range of 10-1000 microg l(-1) and detection limits for the target compounds were between 1.2 and 11.8 microg l(-1) depending on which detector was used. The method was applied for determining fenitrothion and both its metabolites in river waters which run through forest areas near to aerial application of the pesticide.

Chromatography, High Pressure Liquid↗

PubMed2004

Optimization and validation of a method of analysis for fenitrothion and its main metabolites in forestry air samples using sorbent tubes with thermal desorption cold trap injection and gas chromatography-mass spectrometry.

An analytical methodology using thermal-desorption cold trap (TCT) and GC-MS was developed for the determination of the insecticide fenitrothion and its main metabolites, 3-methyl-4-nitrophenol and fenitrooxon, in forestry atmospheres. The sampled atmosphere was pumped through a glass tube containing 100 mg of Tenax adsorbent at a flow rate of 50 ml min(-1). Adsorption/thermal desorption and breakthrough experiments were performed to test the ability to quantitatively trap the compounds. The detection limits of method for these compounds ranged between 1.6 and 2.1 ng m(-3). This methodology was developed to evaluate the persistence of fenitrothion in forest atmospheres after treatment. Spray application at 21.5 mg active ingredient m(-2) resulted in atmosphere levels of the insecticide of 78.3 ng m(-3) (after 2 h of application). Within 2-4 days following treatment, the presence of fenitrooxon fell to 50-55%. During this period residues of metabolites began to appear, disappearing 19 days later.

Air↗

PubMed2003

Coupling solid-phase microextraction and high-performance liquid chromatography for direct and sensitive determination of halogenated fungicides in wine.

A solid-phase microextraction (SPME) method coupled to high-performance liquid chromatography with diode array detection (HPLC-DAD) for the analysis of six organochlorine fungicides (nuarimol, triadimenol, triadimefon, folpet, vinclozolin and penconazole) in wine was developed. For this purpose, polydimethylsiloxane-divinylbenzene-coated fibers were utilized and all factors affecting throughput, precision, and accuracy of the SPME method were investigated and optimized. These factors include: matrix influence, extraction and desorption time, percentage of ethanol, pH, salt effect and desorption mode. The performed analytical procedure showed detectability ranging from 4 to 27 microg l(-1) and precision from 2.4 to 14.2% (as intra-day relative standard deviation, RSD) and 4.7-25.7% (as inter-day RSD) depending on the fungicide. The results demonstrate the suitability of the SPME-HPLC-DAD method to analyze these organochlorine fungicides in red wine.

Chromatography, High Pressure Liquid↗

PubMed2001

VLDL modulates the cytokine secretion profile to a proinflammatory pattern.

Human very-low-density lipoprotein (VLDL) inhibits DNA synthesis in lymphocytes activated by the nonspecific mitogen concanavalin A (Con A). We studied the effects of VLDL on lymphocyte activation (IL-2 receptor expression), cell cycle progression, and production of IL-2 and of IL-4 (a proinflammatory and an anti-inflammatory interleukin, respectively) to understand why an atherogenic lipoprotein inhibits cell proliferation. After 48 h of stimulation with the mitogen, VLDL decreased the population of cells bearing IL-2 receptor and the population of T-cells that progress through the cell cycle, increasing the population of T-cells in G(0)/G(1). Cells cultured in the presence of Con A and VLDL produced higher levels of IL-2 and lower levels of IL-4 than cells cultured without VLDL. These results suggest that VLDL inhibits lymphocyte proliferation by reducing IL-2 receptor and enhancing the levels of IL-2. Probably, one atherogenic effect of VLDL is to modulate the cytokine secretion profile of lymphocytes to a predominantly proinflammatory response.

Animals↗

PubMed2001

Multimembrane carbon fiber microelectrodes for amperometric determination of serotonin in human urine.

An electrochemical sensor for the determination of serotonin in urine was prepared using Ni(II)-phthalocyanine and Nafion to modify the surface of a 4 mm length carbon fiber microelectrode. The resultant sensor was found to improve the response towards this neuronal amine versus the microelectrode without the polymer films. Different polymerization conditions, as well as different conditioning solutions and buffer systems, were investigated in order to optimize the response of the electrodes. Square wave voltammetry (SWV) is proposed as a direct method for determination of serotonin in human urine, after a solid-liquid extraction process. The proposed method enables a detection limit for serotonin of 0.80 +/- 0.04 microgram L-1 to be achieved at a reduction potential of 0.35 V, with an overall prediction error of 2.2% and recoveries of 93%.

Carbon↗

PubMed2000

Solid-phase microextraction for the determination of systemic and non-volatile pesticides in river water using gas chromatography with nitrogen-phosphorous and electron-capture detection.

A solid-phase microextraction (SPME) method combined with gas chromatography with nitrogen-phosphorous and electron capture detection for the analysis of the pesticides terbumeton, metribuzine, isomethiozine, pyridafenthion and triadimenol in river water has been developed. For this purpose, polyacrylate and polydimethylsiloxane coated fibres have been utilised and the factors affecting throughput, precision and accuracy of the SPME method have been investigated and optimised. These factors include: matrix influence, adsorption time, pH, salt effect, desorption time, temperature and also the lapse of time between sampling and injection. The performed analytical procedure showed detectability ranging from 2.0 ng l(-1) to 3.0 microg l(-1) and precision from 1.9 to 27.7% (as relative standard deviation) depending on the pesticide, the fibre and the detector used. The results demonstrate the suitability of the SPME method to analyse these non-volatile pesticides in river water.

Chromatography, Gas↗

PubMed1998

Determination of the insecticide pyridafenthion in river water, soils and wine by adsorptive stripping voltammetry.

Solid-phase extraction or liquid-liquid extraction has been combined with adsorptive stripping voltammetry at a hanging mercury drop electrode to isolate, determine, quantify and recover trace concentrations of pyridafenthion in water, wine and soil. A systematic study of the experimental parameters affecting the stripping response was carried out by differential pulse voltammetry. By using an accumulation potential of 400 mV and an accumulation time of 540 s, the limit of detection was 0.17 microgram l-1 and the relative standard deviation (n = 10) was 1.9% at a concentration level of 8.5 micrograms l-1. Different methods are proposed which eliminate matrix interferences. These results have been applied to the systematic study of this compound in water, wine and soil. The lowest detectable concentration for pyridafenthion is 34 micrograms l-1 in water, 102 micrograms l-1 in wine and 80 micrograms kg-1 in soil. Recoveries of the pyridafenthion from supplied environmental samples were in all cases higher than 92% with a relative standard deviation lower than 3%.

Electrochemistry↗