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1.
Talanta ; 142: 124-30, 2015 Sep 01.
Article in English | MEDLINE | ID: mdl-26003701

ABSTRACT

A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min.


Subject(s)
Insecticides/analysis , Permethrin/analysis , Phenylcarbamates/analysis , Water Pollutants, Chemical/analysis , Chromatography, High Pressure Liquid , Czech Republic , Environmental Monitoring , Lakes/analysis , Online Systems , Rivers/chemistry , Solid Phase Extraction
2.
Environ Sci Pollut Res Int ; 21(6): 4286-96, 2014 Mar.
Article in English | MEDLINE | ID: mdl-24306720

ABSTRACT

The study describes the environmental monitoring of anionic surfactants-alcohol sulfates (AS) and alcohol ethoxysulfates (AES)-in marine sediments. Concentration values were obtained after pressurised liquid extraction (PLE) and liquid chromatography-tandem mass spectrometry analysis (LC-MS/MS). Samples were collected from a range of wastewater discharge points along the coast of the provinces of Huelva, Málaga, Granada and Almería. Urban, agricultural and industrial wastewaters are discharged at the selected 38 sampling sites. Principal component analysis was carried out in order to evaluate the distribution and behaviour of these compounds in these coastal environments. Evaluation of the data revealed that the behaviour and sources of AS and AES in marine sediments are different, and that the distribution of AES depends on the length of the alkyl chain, while the number of ethoxylated units is not relevant. Additionally, the 38 sampling sites can be grouped into only two types of outfalls according to their AS distribution. The concentration of compounds in sediment samples ranged from 7.52 to 13.50 mg kg(-1) for AS, from 3.04 to 10.68 mg kg(-1) for AES-C12Ex and from 3.83 to 11.56 mg kg(-1) for AES-C14Ex.


Subject(s)
Alcohols/analysis , Environmental Monitoring , Geologic Sediments/chemistry , Sulfates/analysis , Surface-Active Agents/analysis , Water Pollutants, Chemical/analysis , Agriculture/statistics & numerical data , Chromatography, Liquid , Mass Spectrometry , Tandem Mass Spectrometry , Wastewater/chemistry , Wastewater/statistics & numerical data
3.
Environ Toxicol Chem ; 33(3): 508-15, 2014 Mar.
Article in English | MEDLINE | ID: mdl-24288239

ABSTRACT

Alcohol sulfates are one of the most important types of commercial anionic surfactants and may pose serious environmental problems. The present study examines the sorption behavior of alcohol sulfates in an agricultural soil using a batch reactor and column experiments. Kinetics and equilibrium isotherms of the sorption and desorption processes of the following alcohol sulfate homologues have been determined: AS-C12, AS-C14, AS-C16 , and AS-C18. Sorption and desorption occurred rapidly, and equilibrium was achieved in approximately 1 h. The sorbed mass percentages were 35.1% AS-C12 , 67.2% AS-C14 , and 100% for both AS-C16 and AS-C18. A pseudo-first-order kinetic model provided an adequate fit of data. Sorption and desorption equilibrium data were fitted into 1) a linear model, with r(2) values in the ranges 0.712 to 0.988 and 0.736 to 0.983, respectively, and 2) a Freundlich model, with r(2) values in the ranges 0.956 to 0.991 and 0.891 to 0.981, respectively. Continuous-flow experiments in soil columns were carried out to obtain the breakthrough curves for each compound. The present study provides basic theoretical concepts and key parameters for developing mathematical models that simulate the migration of alcohol sulfate into agricultural soils.


Subject(s)
Fatty Alcohols/chemistry , Soil Pollutants/chemistry , Soil/chemistry , Sulfuric Acid Esters/chemistry , Surface-Active Agents/chemistry , Adsorption , Agriculture , Kinetics , Models, Theoretical
4.
Prog Neuropsychopharmacol Biol Psychiatry ; 30(6): 1136-8, 2006 Aug 30.
Article in English | MEDLINE | ID: mdl-16762472

ABSTRACT

Studies have shown an association between the T102C polymorphism of the 5HT2a receptor gene and schizophrenia. However, negative findings have also been reported. We conducted a case-control study of the T102C polymorphism in Spanish Caucasians. We compared T102C polymorphism genotypes and allele frequencies in 188 schizophrenia patients and 440 healthy controls. There were significant differences in the distribution of the three genotypes (TT, TC and CC) and in the allele frequencies in controls and schizophrenics. The C allele was more frequent in schizophrenia patients than in healthy controls. The Cochrane-Armitage test for trend indicated a significant dosage effect for schizophrenia of the risk allele (C).


Subject(s)
Polymorphism, Genetic/genetics , Receptor, Serotonin, 5-HT2A/genetics , Schizophrenia/genetics , Adult , Alleles , Case-Control Studies , DNA/genetics , Female , Gene Dosage , Genotype , Humans , Male , Reverse Transcriptase Polymerase Chain Reaction , Risk , Schizophrenia/epidemiology , Schizophrenia/metabolism , Spain/epidemiology
5.
Mem. Inst. Oswaldo Cruz ; 95(5): 641-7, Sept.-Oct. 2000. tab, graf, ilus
Article in English | LILACS | ID: lil-267892

ABSTRACT

A protozoan flagelate has recently been isolated from Amaranthus retroflexus. This plant grows near economically important crops in southeastern Spain, which are known to be parasitized by Phytomonas spp. The present study focuses on the characterization of the energy metabolism of this new isolate. These flagellates utilize glucose efficiently as their primary energy source, although they are unable to completely degrade it. They excrete ethanol, acetate, glycine, and succinate in lower amount, as well as ammonium. The presence of glycosomes was indicated by the early enzymes of the glycolytic pathway, one enzyme of the glycerol pathway (glycerol kinase), and malate dehydrogenase. No evidence of a fully functional citric-acid cycle was found. In the absence of catalase activity, these flagellates showed significant superoxide dismutase activity located in the glycosomal and cytosolic fractions. These trypanosomes, despite being morphologically and metabolically similar to other Phytomonas isolated from the same area, showed significant differences, suggesting that they are phylogenetically different species.


Subject(s)
Animals , Plants/parasitology , Trypanosomatina/metabolism , Energy Metabolism , Superoxide Dismutase/metabolism , Trypanosomatina/chemistry , Trypanosomatina/isolation & purification
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