Biomedical subjects

N Unceta

Publications and source records attributed to N Unceta.

5 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↗

PubMed2005

Speciation of volatile aromatic and chlorinated hydrocarbons in an urban atmosphere using TCT-GC/MS.

Several aromatic and chlorinated volatile hydrocarbons (VOCs) were measured in Vitoria-Gasteiz City (Spain) throughout the years 1999 and 2002 in order to find out the concentration of these pollutants in urban air. These VOCs were retained in Tenax TA, subsequently desorpted by using a thermal desorption cold trap injector (TCT), and thereafter analyzed by gas chromatography/mass spectrometry (GC/MS). This analytical methodology permits the determination of 42 VOCs at very low concentrations, although only 32 of them were found in the urban air of the city (ranging from 205.51 to 0.01 microg m(-3)), with high reproducibility (%RSD lower than 10%). Twenty-four-hour samples were taken each sampling day to ascertain their total daily concentration, and rigorous quality controls were carried out to check the representativeness of sampling. Results of this exhaustive study show that toluene (T), xylenes (X), ethylbenzene (E), and benzene (B) were, respectively, the most abundant of these VOCs in the urban area during that period. The total concentration of BTEX represented, on average, more than 72.6% of the VOC total concentration, with the highest concentrations being reached in autumn, except for benzene and derived compounds (in winter). Benzene was the minority BTEX pollutant, its yearly mean concentration being less than the maximum established by the European Directive 2000/69/CE (5 microg m(-3)).

Air Pollutants↗

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

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↗