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At least 361 records · Page 20Linked to original sources
PubMed2004

First evidence of endocrine disruption in feral carp from the Ebro River.

Feral carps (Cyprinus carpio) were collected in spring 2001 from five sites along the lower course of Ebro River (Spain) with the aim of investigating the existence of endocrine-disrupting effects. Several findings (low gonadosomatic index (GSI), plasmatic vitellogenin (VTG), depressed levels of testosterone, and histological alterations in gonads) detected in male carps downstream of Zaragoza's sewage treatment plant (STP) strongly suggest that the concentration of sewage effluent in the area is a major causal factor leading to the detected estrogenic effects. Important alterations (viz. delayed maturation in females, indications of arrested spermatogenesis in males) were detected in carps from Flix, a heavily industrialized area. Low ovarian P-450 aromatase and reduced glucuronidation of testosterone and estradiol in males were observed in Zaragoza and Canal Imperial de Aragón-an agricultural area-which suggest decreased estrogen synthesis, and possibly, reduced sex hormone excretion in those organisms. These results were related to some in vitro assays aimed to assess the interference of model compounds (atrazin, vinclozolin, diuron, pp'-DDE, dicofol, triphenyltin, nonylphenol, and fenarimol) with the glucuronidation of testosterone and estradiol by liver microsomal fractions. The fungicide fenarimol (10-20 microM) and nonylphenol (50 microM) were found to significantly inhibit (20%) both activities at relatively low doses. Overall, this work provides the first evidence of the existence of significant alterations of the endocrine system of carps from the medium-low course of the Ebro River and demonstrates the ability of several chemicals to modulate the inactivation of endogenous steroids.

Animals↗
PubMed2000

Application of liquid chromatography with mass spectrometry combined with photodiode array detection and tandem mass spectrometry for monitoring pesticides in surface waters.

Liquid chromatography with photodiode array detection (LC-DAD) and liquid chromatography with mass spectrometry (LC-MS) are two techniques that have been widely used in monitoring pesticides and their degradation products in the environment. However, the application of liquid chromatography with tandem mass spectrometry (LC-MS-MS) for such purposes, once considered too costly, is now gaining considerable ground. In this study, we compare these methods for the multi-residue analysis of pesticides in surface waters collected from the central and southeastern regions of France, and from the St. Lawrence River in Canada. Forty-eight pesticides belonging to eight different classes (triazine, amide, phenylurea, triazole, triazinone, benzimidazole, morpholine, phenoxyalkanoic), along with some of their degradation products, were monitored on a regular basis in the surface waters. For LC-MS, we used the electrospray ionization (ESI) interface in the negative ionization mode on acidic pesticides (phenoxyalkanoic, sulfonylurea), and the atmospheric pressure chemical ionization (APCI) interface in the positive ionization mode on the remaining chemicals. Different extraction techniques were employed, including liquid-liquid extraction with dichloromethane, and solid-phase extraction using C18-bonded silica and graphitized carbon black cartridges. Eleven of the target chemicals (desethylatrazine, desisopropylatrazine, atrazine, simazine, terbuthylazine, metolachlor, carbendazime, bentazone, penconazole, diuron and isoproturon) were detected by LC-MS at concentrations ranging from 20 to 900 ng/l in the surface waters from France, and six pesticides (atrazine, desethylatrazine, desisopropylatrazine, cyanazine, simazine and metolachlor) were detected by LC-MS and LC-MS-MS at concentrations ranging from 3 to 52 ng/l in the samples drawn from the St. Lawrence River. There was good correlation between the LC-DAD and LC-MS techniques for 60 samples. The slope of the curves expressing the relationship between the results obtained with LC-DAD versus those obtained by LC-MS was near 1, with a correlation coefficient (r) of over 0.93. The identification potential of the LC-MS technique, however, was greater than that of the LC-DAD; its mass spectra, mainly reflecting the pseudomolecular ion resulting from a protonation or a deprotonation of the molecule, was rich in information. The LC-MS-MS technique with ion trap detectors, tested against the LC-MS on 10 surface water samples, gave results that correlated well with the LC-MS results, albeit generating mass spectra that yielded far more information about the structure of unknown substances. The sensitivity of the LC-MS-MS was equivalent to the selected ion monitoring (SIM) acquisition mode in LC-MS. The detection limits of the target pesticides ranged from 20 to 100 ng/l for the LC-MS technique (under full scan acquisition), and from 2 to 6 ng/l for LC-MS-MS. These limits were improved by a factor of almost 10 by increasing the sample volume to 10 l.

Chromatography, Liquid↗
PubMed2001

Determination of phenylurea herbicides in natural waters at concentrations below 1 ng l(-1) using solid-phase extraction, derivatization, and solid-phase microextraction-gas chromatography-mass spectrometry.

A procedure is presented which allows the ultratrace level determination of phenylurea herbicides (PUHs) in natural waters. Samples were enriched by solid-phase extraction (SPE) on Carbopack B and alkylated with iodoethane and sodium hydride to yield thermostable products. After derivatization, the aqueous samples were extracted and injected by SPME. The use of iodoethane instead of iodomethane allowed the differentiation between parent compounds and the N-demethylated metabolites. Limits of detection were between 0.3 and 1.0 ng/l for the parent compounds. Standard deviations below 10% were achieved for samples containing more than 4 ng/l in very different matrices including Nanopure water, lake water, and waste water treatment plant (WWTP) effluent. Moreover, the para-hydroxylated metabolite of diuron could be quantified with the same procedure. The presence of further metabolites was assessed qualitatively. Chromatography was stable over a large number of measurements even with dirty samples from WWTP effluent. The precision and sensitivity of the developed analytical method allowed the investigation of the fate of PUHs in lakes, their degradation during drinking water treatment and their transport within the North Sea.

Calibration↗
PubMed2001

On the signal response of various pesticides in electrospray and atmospheric pressure chemical ionization depending on the flow-rate of eluent applied in liquid chromatography-tandem mass spectrometry.

The API-MS signal response of several pesticides (atrazine, simazine, isoproturon, diuron, chlorfenvinphos, chlorpyrifos, alachlor, trifluralin) depending on the flow-rate of eluent entering the MS interface was investigated. The investigations were based on API-MS-MS analyses of standard pesticide mixtures in the flow injection mode (FIA) at systematically varied eluent flow-rates using both an ESI interface (Turboionspray) and a heated nebulizer type APCI source. In the result, the individual compounds included in this study showed significant differences in their signal response behaviour depending on the flow-rate of eluent applied. The most hydrophobic compounds among the investigated pesticides (chlorpyrifos and trifluralin) showed drastic losses of sensitivity with increasing eluent flow-rate in both ESI and APCI, while more hydrophilic compounds like atrazine, simazine and isoproturon showed the expected signal response (concentration-sensitive in ESI, mass-flow-sensitive in APCI) at least within a certain range of flow-rates (200-600 microl/min in ESI, 200-2000 microl/min in APCI). These findings lead to the conclusion that application of a programmed HPLC eluent flow-rate may be advantageous to achieve maximum sensitivity of API-MS detection for all pesticides of interest. This is exemplified by the implementation of a flow gradient into an online SPE-HPLC-APCI-MS/MS method for improved analysis of pesticides in drinking water.

Atmospheric Pressure↗
PubMed2002

Poly(methyloctadecylsiloxane) immobilized on silica by gamma radiation for use in solid-phase extraction.

This work presents a fast, easy and effective procedure to obtain silica-based C18 type sorbents for use in solid-phase extraction (SPE). The solid-phase was made by depositing a polymer, poly(methyloctadecylsiloxane) (PMODS), on the silica support followed by immobilization using gamma irradiation. The method presents an application of green chemistry in the analytical laboratory, since there are no toxic residues after the synthesis. Water samples spiked with a mixture of pesticides (benomyl, tebuthiuron, diuron, simazine, atrazine and ametryn) were extracted in the off-line mode in order to evaluate the performance of this sorbent.

Absorption↗
PubMed2003

Investigation of preconcentration strategies for the trace analysis of multi-residue pesticides in real samples by capillary electrophoresis.

In this work, on-line preconcentration strategies were investigated for the multi-residue analysis of pesticides in drinking water and vegetables using micellar electrokinetic chromatography. Among the on-line strategies, sweeping and stacking with reverse migration of micelles (SRMM), with and without the insertion of a plug of water before sample injection, were contrasted. A new version of SRMM was also introduced. The modification consisted of momentarily applying a positive voltage at the inlet vial right after sample has been injected, increasing the efficiency by which the analytes are captured. Nine pesticides from different classes, carbendazim (benzimidazole), simazine, atrazine, propazine and ametryn (triazine), diuron and linuron (urea), carbaryl and propoxur (carbamate), were baseline separated in less than 6 min with a electrolyte composed of 20 mmol l(-1) phosphate buffer at pH 2.5, containing 25 mmol l(-1) sodium dodecyl sulfate and 10% methanol. Limits of detection (LODs) in the order of 2-46 microg l(-1) for the pesticides under investigation were obtained solely using the on-line strategies. Enrichment factors of 3-18-fold were obtained. These factors were computed as the improvement of the concentration LODs with respect to the reference condition (injection of 10 s at 2.5 kPa pressure). The proposed methodologies were applied to the analysis of pesticides in complex matrices such as carrot extracts where the detection of 2.5 microg l(-1) was illustrated. By combining off-line solid-phase extraction and the proposed on-line strategies, the detection of pesticides in drinking water at the 0.1 microg l(-1) level was conceived.

Electrophoresis, Capillary↗
PubMed1997

Rapid target analysis of microcontaminants in water by on-line single-short-column liquid chromatography combined with atmospheric pressure chemical ionization tandem mass spectrometry.

The applicability of trace enrichment and separation of microcontaminants on a 10 mm x 2 mm I.D. high-pressure packed (8 microns C18 bonded silica or 10-15 microns PLRP-S) column combined on-line with an atmospheric pressure chemical ionization MS-MS system is demonstrated for the target analysis of herbicides in river water. Tailor-made procedures are obtained for a limited number of analytes by tuning the chromatographic efficiency of the short LC column and the specificity of tandem MS, in order to minimize the analysis time. With the on-line short-column LC-MS-MS method, good linearity is obtained for the herbicides in the range of 0.1-10 micrograms/l. The relative standard deviations of peak areas are less than 5% and, with only 4-ml samples, detection limits of 0.01-0.1 microgram/l can be achieved. The total analysis time is 10-15 min. The 10 mm x 2 mm I.D. LC columns packed with 8 microns particles show good stability and can be used for at least 40 analyses. Target compound analyses of river water allowed the confirmation of the presence of herbicides such as diuron, simazine, atrazine and terbutylazine at sub-microgram/l levels.

Chromatography, High Pressure Liquid↗
PubMed1998

Simultaneous quantitative determination of thirteen urea pesticides at sub-ppb levels on a Zorbax SB-C18 column.

A simple multi-residue method is described for simultaneously determining ten urea and three benzoylurea pesticides residues in drinking water with quantitation limits below the European regulatory limit of 0.1 microgram/l. The residues were extracted from drinking water with dichloromethane and analysed by HPLC on a Zorbax 5 microns SB-C18 column with diode array detection (DAD) at 240 nm. Recoveries were determined by spiking drinking water with 13 pesticides (benzthiazuron, metoxuron, monuron, fluometuron, isoproturon, diuron, linuron, chloroxuron, chlorbromuron, diflubenzuron, neburon, triflumuron and flucycloxuron) at the 0.05-0.50 microgram/l level.

Chromatography, High Pressure Liquid↗
PubMed1999

Ultra-trace-level determination of polar pesticides and their transformation products in surface and estuarine water samples using column liquid chromatography-electrospray tandem mass spectrometry.

A method is developed for the determination of polar pesticides and their transformation products [atrazine, deethylatrazine, deisopropylatrazine, hydroxyatrazine, diuron, 3,4-dichlorophenylmethylurea, 3,4-dichlorophenylurea (DPU), monuron, bentazone, anthranil-isopropylamide, chloridazon, metolachlor] in surface, estuarine and sea water samples at the low ng/l level. Solid-phase extraction is combined off-line with column liquid chromatography-electrospray ionization tandem mass spectrometric detection (LC-ESI-MS-MS). The applicability of two solid-phase materials, i.e., LiChrolut EN cartridges and graphitized carbon black extraction disks, is evaluated. The influence of the organic solvent used in gradient LC, as well as the amount of co-extracted humic material on the ESI process is studied. The eluotropic strength of the organic solvent was found to have a distinct effect on the sensitivity of ESI-MS if coupled with LC gradient separations. Methanol gave much better results than acetonitrile and phenylurea compounds are more susceptible to solvent changes than triazines. Co-extracted humic material causes signal suppression in ESI-MS-MS detection. The degree of suppression depends upon the sample pH and the nature of the samples, i.e., surface or estuarine water. Detection limits in LC-ESI-MS-MS ranged from 0.2 to 2 ng/l, with the exception of DPU (8 ng/l). The applicability of the procedure was demonstrated by analyzing surface and estuarine water.

Chromatography, Liquid↗
PubMed2000

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Chromatography, Liquid↗
PubMed2000

Reversed migration micellar electrokinetic chromatography with off-line and on-line concentration analysis of phenylurea herbicides.

Three environmentally important phenylurea herbicides (monuron, isoproturon, diuron) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 50 mM sodium dodecyl sulfate, 50 mM phosphoric acid, and 15 mM gamma-cyclodextrin. Three on-line concentration techniques are then evaluated to increase the detection sensitivity of the RM-MEKC system. Stacking with reverse migrating micelles (SRMM, water as the sample solvent) provided the best results among the focusing techniques studied. Using a z-shaped detection cell, more than 500-fold increase in peak height is obtained. As a sample preparation and off-line concentration method, solid-phase extraction (SPE) that further improved detection sensitivity was used in the analysis of spiked tap and pond water. For example, 1 parts per billion of each herbicide spiked in tap or pond water was detected by MEKC after SPE and SRMM.

Chromatography, Micellar Electrokinetic Capillary↗
PubMed2003

Metabonomics classifies pathways affected by bioactive compounds. Artificial neural network classification of NMR spectra of plant extracts.

The biochemical mode-of-action (MOA) for herbicides and other bioactive compounds can be rapidly and simultaneously classified by automated pattern recognition of the metabonome that is embodied in the 1H NMR spectrum of a crude plant extract. The ca. 300 herbicides that are used in agriculture today affect less than 30 different biochemical pathways. In this report, 19 of the most interesting MOAs were automatically classified. Corn (Zea mays) plants were treated with various herbicides such as imazethapyr, glyphosate, sethoxydim, and diuron, which represent various biochemical modes-of-action such as inhibition of specific enzymes (acetohydroxy acid synthase [AHAS], protoporphyrin IX oxidase [PROTOX], 5-enolpyruvylshikimate-3-phosphate synthase [EPSPS], acetyl CoA carboxylase [ACC-ase], etc.), or protein complexes (photosystems I and II), or major biological process such as oxidative phosphorylation, auxin transport, microtubule growth, and mitosis. Crude isolates from the treated plants were subjected to 1H NMR spectroscopy, and the spectra were classified by artificial neural network analysis to discriminate the herbicide modes-of-action. We demonstrate the use and refinement of the method, and present cross-validated assignments for the metabolite NMR profiles of over 400 plant isolates. The MOA screen also recognizes when a new mode-of-action is present, which is considered extremely important for the herbicide discovery process, and can be used to study deviations in the metabolism of compounds from a chemical synthesis program. The combination of NMR metabolite profiling and neural network classification is expected to be similarly relevant to other metabonomic profiling applications, such as in drug discovery.

Herbicides↗
PubMed2001

Toxicity characterisation of organic contaminants in stormwaters from an agricultural headwater stream in south east England.

The transient movement of pesticides at biologically active concentrations during storm events is considered to be a cause of biological impoverishment in some headwater streams. The programme of work described sought to identify compounds that are the cause of toxic effects during such events. Along with targeted pesticide analysis, toxicity identification evaluation (TIE) procedures were used to identify compounds with a demonstrated toxic effect. These procedures were specifically directed towards isolating and attributing toxicity to classes of organic contaminants in samples collected from an English headwater stream during a storm event. The organic load was isolated by means of solid-phase extraction (SPE). Bioassay of the SPE extract at x 100 whole water concentrations confirmed that the samples contained substances toxic to Daphnia magna, although the raw samples were not toxic. Targeted pesticide analysis identified simazine and diuron as the major pesticides present and, using a toxicity unit (TU) approach. were shown to be responsible for a significant amount of the observed concentrate toxicity during a runoff event. However, they were not present in sufficient quantities to be totally responsible for a more toxic later event. By simplification of the SPE isolate using reverse-phase HPLC, fractions from which were tested for toxicity, the cause of concentrate toxicity in the later event was isolated to two discrete fractions. GC-MS analysis of these fractions identified nonylphenol. endosulfan sulphate and pendimethalin as present, with the majority of toxicity attributed to nonylphenol (NP). The main advantage of the TIE approach is that it allows biological active compounds with a demonstrated effect to be identified that may not be selected by more traditional techniques.

Agriculture↗
PubMed2002

Sources of pesticides in surface waters in Switzerland: pesticide load through waste water treatment plants--current situation and reduction potential.

Concentrations of pesticides in Swiss rivers and lakes frequently exceed the Swiss quality goal of 0.1 microg/l for surface waters. In this study, concentrations of various pesticides (e.g., atrazine, diuron, mecoprop) were continuously measured in the effluents of waste water treatment plants and in two rivers during a period of four months. These measurements revealed that in the catchment of Lake Greifensee, farmers who did not perfectly comply with 'good agricultural practice' caused at least 14% of the measured agricultural herbicide load into surface waters. Pesticides, used for additional purposes in urban areas (i.e. protection of materials, conservation, etc.), entered surface waters up to 75% through waste water treatment plants.

Agriculture↗
PubMed2003

A qualitative sampling method for monitoring water quality in temporary channels or point sources and its application to pesticide contamination.

A water-sampling device to monitor the quality of water periodically and temporarily flowing out of concrete tubes, sewers or channels is described. It inexpensively and easily enables a qualitative characterization of contamination via these point-source entry routes. The water sampler can be reverse engineered with different sizes and materials, once installed needs no maintenance, passively samples the first surge, and the emptying procedure is short. In an agricultural catchment area in Germany we monitored an emergency overflow of a sewage sewer, an outlet of a rainwater sewer and two small drainage channels as input sources to a small stream. Seven inflow events were analysed for 20 pesticide agents (insecticides, fungicides and herbicides). All three entry routes were remarkably contaminated. We found parathion-ethyl concentrations of 0.3 microg l(-1), diuron up to 17.3 microg l(-1), ethofumesate up to 51.1 microg l(-1), metamitron up to 92 microg l(-1) and prosulfocarb up to 130 microg l(-1).

Engineering↗
PubMed1997

Evaluation of ELISA microtiter plate-based assays for the direct determination of isoproturon in water samples and soil extracts.

Trials were carried out on the commercially available Millipore isoproturon ELISA microtiter plate tests and on laboratory assays developed by Hirst as part of a Joint European Union research project (BIOPTICAS). The lowest detectable dose (LDD) was determined as three times the standard deviation of the blanks. Depending on the calibration curves obtained on different days with different plates, the LDD varied from 0.020 to 0.064 microgram/L for the Millipore test and from 0.080 to 0.329 microgram/L for the Hirst test. The mean coefficients of variation within a single plate for triplicate determinations of standard solutions in the 0.05 to 0.5 microgram/L range were 5.5 and 3.6% for Millipore and Hirst respectively. Cross-reactivity was studied for mono- and di-demethylated isoproturon, chlortoluron, diuron and linuron. The highest cross-reactivity with both tests was that of mono-demethylated isoproturon (22% for Millipore, 4% for Hirst). This molecule was the only one to show significant cross-reactivity in the Hirst test, whereas in the Millipore test, the di-demethylated isoproturon also cross-reacted (4%). Natural water samples, 19 ground-, 53 lysimetric plate and 47 suction cup water samples, and 32 soil samples were also analysed with the ELISA tests. HPLC with a diode array detector was used as a validated control technique for the natural samples. For each water type, ELISA concentrations of both tests were significantly correlated with the HPLC values (r > or = 0.937; p < 0.001). For the soil extracts, the correlations were also significant (p < 0.001), but the scatter in the data was greater. Overall, the Millipore correlation coefficients were higher than those of Hirst.

Antibodies↗
PubMed1998

Surface water pollution by herbicides from effluents of waste water treatment plants.

Herbicide loads of urban and rural waste water treatment plant effluents were calculated over a one-year period by measuring the herbicide concentrations in 14-day mixed samples. More than three quarters of the total herbicide load of the effluent of the rural waste water treatment plant consists of isoproturon. Particularly large amounts of this substance contribute to the total herbicide load during the main application in spring and in early autumn. The measured loads of atrazine and the increased ratio between atrazine and desethylatrazine in spring indicate that atrazine is still applied in Germany. More than 80% of the total herbicide load of the effluent of the urban waste water treatment plant consists of diuron which is mainly used in urban weed control. The results show that also effluents of urban waste water treatment plants contribute to a great extent to herbicide pollution of surface water.

Environmental Monitoring↗
PubMed2000

Comparison of atmospheric pesticide concentrations measured at three sampling sites: local, regional and long-range transport.

We present the comparison of atmospheric concentrations of eleven currently used pesticides (HCB, alpha-HCH, gamma-HCH, trifluraline, mecoprop, phosalone, atrazine, carbofuran, carbaryl, diuron and isoproturon) measured in remote (Aubure), rural (Colmar) and urban (Strasbourg) areas of Alsace and Vosges regions (cast France). Pesticides samples were collected simultaneously on two of the three sites during the summer season of 1993 and 1994, using a Hi-Vol sampler with Whatman filter paper and XAD-2 resin. The particle and gas phases were collected separately during 24 h. The relative importance of local emissions and local, regional and long distance transport on the contamination of the atmosphere in the three environments (remote, rural and urban) were investigated. To facilitate the interpretation of the results, the alpha/gamma-HCH ratio was used as a tracer of pesticide emissions.

Air Movements↗