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At least 343 records · Page 19Linked to original sources
PubMed2000

Use of solid-phase extraction and high-performance liquid chromatography for the determination of triazine residues in water: validation of the method.

A method for determination of some triazine residues in water has been developed. The method involves concentration with C18 solid-phase extraction cartridges followed by high-performance liquid chromatographic analysis using a C18 column with UV detection at 230 nm, a mobile phase of methanol-water (60:40, v/v) at pH 4.6 (phosphoric acid) and a flow-rate of 0.8 ml/min. After optimization of the extraction and separation conditions, the method was validated. The method can be used for determination of atrazine, simazine, cyanazine and ametryn in water, within the international limits of 0.1 microg/l.

Chromatography, High Pressure Liquid↗
PubMed2000

Trace-level determination of triazines and several degradation products in environmental waters by disk solid-phase extraction and micellar electrokinetic chromatography.

An analytical method combining disk solid-phase extraction with micellar electrokinetic chromatography has been developed for the determination of atrazine, simazine, hydroxyatrazine, deisopropylatrazine, deethylatrazine, propazine and prometryn in water samples. The influence of the buffer and sodium dodecyl sulfate (SDS) concentration, pH and organic modifier on the separation has been studied. Baseline separation of the seven triazines was achieved under the following conditions: 10 mM borate buffer, 60 mM SDS, 20% methanol and pH 9.2. C18-bonded silica and poly(styrene-divinylbenzene) (PS-DVB) disks were evaluated for solid-phase extraction of the selected pesticides (11 of water sample). Using two PS-DVB disks, quantitative recoveries were obtained for all pesticides tested. The method was successfully applied for the determination of the seven triazines in drinking and well water at the 0.1 microg l(-1) and 0.5 microg l(-1) concentration levels, respectively. The detection limits for these analytes using the proposed analytical method were within the 0.02-0.06 microg l(-1) range in drinking water and the 0.06-0.30 microg l(-1) range in well water.

Buffers↗
PubMed1999

The mammary tumor response in triazine-treated female rats: a threshold-mediated interaction with strain and species-specific reproductive senescence.

Triazine herbicides are among the most heavily used agricultural pesticides. Although they possess a very low acute toxicity in animals, a mammary tumor response has been consistently observed in Sprague-Dawley (SD) female rats following chronic oral dosing of atrazine and simazine at and above maximum tolerated doses. However, a substantial collection of detailed research has clearly shown that triazines are not genotoxic or mutagenic, nor do they possess estrogenic agonist activity that might promote mammary tumor growth. Examination of estrous cycling records of atrazine-treated SD rats revealed a premature appearance of persistent estrous episodes, beyond the prevalent occurrence normally seen in untreated, aging SD rats. A significant correlation has been found between early or severe estrous cycle disruption of atrazine-treated rats and the early appearance of mammary tumors. In studies using SD female rats fed atrazine for 6 months, then ovariectomized and administered an estrogen-containing silastic s.c. implant, a deficient luteinizing hormone surge was observed at a 400 parts per million (ppm) dose, but not at 25 or 50 ppm. Because SD rats exhibiting persistent estrus also have a prolonged elevation of estrogen secretion, it is proposed that the triazine-associated mammary tumor response is promoted by the test animal's own estrogen from ovarian follicles that fail to ovulate because gonadotropin surge sufficiency is blocked by the high dose of herbicide. It is further proposed that, because reproductive senescence in SD rats is fundamentally different from menopause in women, the animal response to dosing, as well as the enormous requisite dosing level, establishes a safety margin of very low risk to human health from this mode of action.

Aging↗
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↗
PubMed2003

Comparison of nutrient and contaminant fluxes in two areas with different hydrological regimes (Empordà Wetlands, NE Spain).

Nutrient (N and P), heavy metal (Ni, Cd, Cr, Cu and Pb) and pesticide (DDT, DDD, DDE, lindane, aldrin, endrin, dieldrin, permethrin, atrazine and simazine) concentrations in water and sediment were analysed in the Empordà Wetlands, a Mediterranean wetland area in NE Spain. Mean nutrient and contaminant concentrations and input and output loads via tributaries were compared in two marshes with different water turnover: a freshwater marsh (FWM), with a high water turnover rate due to continuous surface water inputs and outputs, and a brackish water marsh (BWM), with lower turnover and no continuous surface output, where water remains confined during dry periods. Mean concentrations of most heavy metals exceeded the maximum permissible concentration (MPC) in BWM, whilst only some pesticides reached MPC in FWM. The confined waters of BWM showed higher sensitivity to contaminant input loadings than FWM due to the lack of continuous water outputs. Non-point source pollution inputs during runoff (mainly in FWM) and concentration during confinement (mainly in BWM) showed as the main environmental problems related to nutrients and contaminants in these ecosystems. Thus, the importance of confinement and its effect on pollutant concentrations must be borne in mind to achieve correct management of Mediterranean wetlands.

Ecosystem↗
PubMed2003

Evaluation of pesticide uptake by Lupinus seeds.

Pesticide uptake by seeds depends on the properties of the chemical, such as structure, stability, log k(ow) and diffusion rate, type of water, pH, temperature, content of organic matter and composition, and on seed characteristics such as permeability of the seed coat. The efficiency with which Lupinus angustifolius seeds retain different herbicides (simazine, atrazine, isoproturon, linuron,) and insecticides (carbaryl, fenamiphos, permethrin) was evaluated using both a batch and a continuous system. Factors which affect pesticide uptake by seeds, such as flow rate, seed biomass, pesticide concentration, contact time, pH, seed saturation and also the speed of the retention process for 17 days, were tested. L. angustifolius showed a high retention capacity for the above mentioned pesticides. The extraction of pesticides from seeds using different organic solvents, such as methanol, acetonitrile, ethyl acetate and n-hexane was evaluated and no pesticide residues were detected in any of the solvents tested. This could be attributed to the capacity of the seed to degrade the pesticides. From the results obtained, L. angustifolius seems to be a promising seed to be applied for phytoremediation of industrial effluents or contaminated water.

Biodegradation, Environmental↗
PubMed2003

Effect of natural organic matter on powdered activated carbon adsorption of trace contaminants: characteristics and mechanism of competitive adsorption.

Batch adsorption experiments using powdered activated carbon (PAC) to remove trace synthetic organic chemicals (SOCs) from water containing natural organic matter (NOM) were conducted. The percentage of SOC removed at any contact time and at any PAC dose was observed to be independent of the initial SOC concentration. Equations derived from the ideal adsorbed solution theory and the pore surface diffusion model validated this observation. For the strongly adsorbing SOCs (simazine and simetryn), the percentage of SOC removed was independent only at low initial SOC concentrations. The NOM fraction competing with the weakly adsorbing SOC (asulam) constituted a larger percentage of the total NOM than that competing with the strongly adsorbing SOCs. Although the adsorptive capacities of the SOCs were greatly reduced in water containing NOM compared with those in pure water, the change in the pore diffusion coefficient was insignificant. Therefore, NOM competed with the SOCs for adsorption sites, reducing the adsorptive capacity, but the amount of NOM loading was not so severe that it blocked or filled the pores, hindering the internal diffusion of the SOCs.

Adsorption↗
PubMed2003

Calcium accumulation on activated carbon deteriorates synthetic organic chemicals adsorption.

The accumulation of calcium on biological activated carbon (BAC) and their effects on adsorption of synthetic organic chemicals (SOCs) were studied using BAC, which have been operated for 5 (BAC5.0) and 3.5 (BAC3.5) years in a pilot-scale water purification plant, and granular activated carbon (GAC) preloaded with fulvic acid and/or calcium. The major inorganic material accumulated on BAC was calcium. The amounts of calcium on BAC5.0 and BAC3.5 were 36.6 and 29.7 mg g(-1), respectively. Seventy-one percent of calcium existed as calcium carbonate in both BACs. BAC5.0 had higher amount of accumulated calcium than BAC3.5 even though both BACs have already exhausted for NOM in the influent in 1-year operation, suggesting that calcium carbonate gradually accumulated on BAC even after the 3.5 years of operation. The isotherms of GAC preloaded with fulvic acid and/or calcium clearly indicated that the calcium accumulation on GAC reduced adsorption capacity for simazine. The conclusion also confirmed by significant recovery of adsorption capacity of both BACs by acid-washing to remove accumulated calcium from BACs. The difference of adsorption capacity between BAC3.5 and BAC5.0 was caused not only by the difference of adsorbed NOM but also the difference in the amount of accumulated calcium.

Adsorption↗
PubMed2002

Triazines in the aquatic systems of the Eastern Chinese Rivers Liao-He and Yangtse.

The results of a one-year monitoring program on the two Eastern Chinese River systems, i.e. the Liao-He and the Yangtse, with special emphasis on the presence of triazine herbicides are presented. Sediment, suspended solids and water samples from both rivers were analyzed. Additionally, recovery experiments on the SPE-in-field-enrichment procedure and the extraction methods were performed. The samples were measured by gas chromatography coupled with mass spectrometry, electron capture detection and a newly developed mu-plasma atomic emission detector. A typical result of a one-year monitoring was obtained in case of the Liao-He: During winter, at low water period, low triazine values were found. A similar situation was found in early spring. Highest concentrations of atrazine up to 1600 ng/l were found in late spring in the water samples. Maximum concentrations of atrazine, simazine, propazine, simetryn and prometryn were observed in this season as a result of the actual use of triazines. Finally, after the high water period in autumn the triazine concentrations decreased. Additionally, atrazine adsorbed on sediment (up to 2.8 ng/g) and suspended solids was determined (up to 8 ng/l) during late spring sampling. Therefore, the logarithm of the organic carbon based sorption coefficient of atrazine could be calculated. Low levels of atrazine were measured in the water of Yangtse (up to 18.3 ng/l). The concentrations from all sampling points and sampling stations of a particular sampling date were similar, which indicates a homogeneous distribution of this herbicide. Due to the high discharge rate of up to 79,000 m3/s in case of the Yangtse a considerable mass transport of up to 57.5 kg per day atrazine may take place, even at concentrations below the European drinking water limit of 100 ng/l.

Adsorption↗
PubMed2003

Gas chromatography/mass spectrometry applied for the analysis of triazine herbicides in environmental waters.

The excess use of triazine herbicides in agriculture causes severe contamination to the environment especially for ground water. Gas chromatography coupled with mass spectrometry (GC/MS) was used to analyze simazine, atrazine (ATR), cyanazine, as well as the degradation products of ATR such as deethylatrazine and deisopropylatrazine in environmental water samples. These compounds were baseline separated by the established GC method. The water samples were pre-concentrated by solid-phase-extraction (SPE) and analyzed by ion trap MS at sub- to low-ppt levels. Recovery of ATR by the SPE pre-concentration using a C18 cartridge was determined as 90.5 +/- 3.5%. Detection limit of the method using selected ion monitoring technique for ATR was 1.7 ppt when one liter water was analyzed. The relative analytical error for ATR fortified water samples at 200 ppt was -12.5% (n=12) with triple analysis and the relative standard deviation was 3.2%. Trace levels of ATR at 3.9 and 9.7 ppt were determined in water samples collected from a reservoir and a river in Hong Kong.

Atrazine↗
PubMed1998

Occurrence of pesticides in Danish shallow ground water.

Shallow ground water from four different catchment areas, two sandy and two clayey locations, were investigated for content of pesticides and -degradation products. The samples were taken from screens in extraction wells placed from 1.5 to 5 meters below surface 46 different compounds were included in the study, and the analysis were performed with liquid chromatography mass spectrometry (LC-MS) with detection limits below 0.01 microgram/L. In total more than 300 samples were analysed and the most frequently found compounds being atrazine and its degradation products, bentazone, MCPA, metamitron, isoproturon and simazine. 23 out of the 46 compounds were detected in one or more samples. Four different sulfonylurea herbicides were included in the study as they to some extent have substituted phenoxyacid herbicides in agricultural practice and in much lower dosage. Sulfonylurea herbicides did not occur in any samples.

Agriculture↗
PubMed1999

A field study to compare performance of stainless steel research monitoring wells with existing on-farm drinking water wells in measuring pesticide and nitrate concentrations.

Existing drinking water wells are widely used for the collection of ground water samples to evaluate chemical contamination. A well comparison study was conducted to compare pesticide and nitrate-N data from specially designed stainless steel research monitoring wells with data from nearby existing on-farm drinking water wells. Results could help to determine whether adequate information concerning ground water contamination can be obtained from existing drinking water wells for use in making pollutant control decisions. The study was conducted during 1993-1994 in the Little Coharie Watershed, a 158 square mile area located in the coastal plain of eastern North Carolina. Statistical analysis indicated that research monitoring wells provided a greater probability of detecting pesticides in ground water than existing on-farm wells. Atrazine was the most frequently detected pesticide found in all wells, followed in order by fluometuron, carbofuran, metolachlor, alachlor, carbaryl, butylate, chlorothalonil, linuron and simazine. Ninety-seven percent of all wells had observed concentrations of nitrate-N, ranging from 0.1 to 30.1 mg/L. There was not a significant difference between research wells and existing wells for monitoring nitrate-N. Based on results of this study, existing drinking water wells can be used for monitoring nitrate; however, specialized stainless steel monitoring wells should be used for monitoring pesticides in ground water.

Databases, Factual↗
PubMed2002

Detection of estrogenic activity in sediment-associated compounds using in vitro reporter gene assays.

Sediments may be the ultimate sink for persistent (xeno-)estrogenic compounds released into the aquatic environment. Sediment-associated estrogenic potency was measured with an estrogen receptor-mediated luciferase reporter gene (ER-CALUX) assay and compared with a recombinant yeast screen. The ER-CALUX assay was more sensitive to 17beta-estradiol (E2) than the recombinant yeast screen, with an EC50 of 6 pM E2 compared to 100 pM in the yeast screen. Yeast cells were unable to distinguish the anti-estrogens ICI 182,780 and (4-hydroxy)tamoxifen, which were agonistic in the yeast. Acetone-soluble fractions of hexane/acetone extracts of sediments showed higher estrogenic potency than hexane-soluble extracts in the ER-CALUX assay. Sediments obtained from industrialized areas such as the Port of Rotterdam showed the highest estrogenic potency of the 12 marine sediments tested (up to 40 pmol estradiol equivalents per gram sediment). The estrogenic activity of individual chemicals that can be found in sediments including: alkylphenol ethoxylates and carboxylates; phthalates; and pesticides, was tested. Increasing sidechain length of various nonylphenol ethoxylates resulted in decreased estrogenic activity. Of the phthalates tested, butylbenzylphthalate was the most estrogenic, though with a potency approximately 100,000 times less than E2. The organochlorine herbicides atrazine and simazine failed to induce reporter gene activity. As metabolic activation may be required to induce estrogenic activity, a metabolic transformation step was added to the ER-CALUX assay using incubation of compounds with liver microsomes obtained from PCB-treated rats. Results indicate that metabolites of E2, NP and bisphenol A were less active than the parent compounds, while metabolites of methoxychlor were more estrogenic following microsomal incubations.

Animals↗
PubMed1998

Spatial and temporal variations of herbicide (triazines and phenylureas) concentrations in the catchment basin of the Marne river (France).

Triazine and phenylurea concentrations were investigated in four sub-basins of the Marne river (France) in 1992 and 1993. The peak concentrations of atrazine, simazine and isoproturon occurred between March and July. In the four basins, the peaks were in relation with the herbicide application periods and with the important rainfalls, except for the isoproturon. The peaks of terbutryne and ametryne came later in the year, due to their use for weed control on post-emergent corn. For the phenylureas, the peak concentrations were observed in March-April next to the spraying period on winter cereals. The fast transfer of those herbicides was related to their high water solubility. In all the samples, the deethylatrazine (DEA) was detected 1 month after the atrazine due to its degradation within the soils which is of minor importance as compared to its transport by surface waters and also, to interactions between the silt sheet and the stream itself. The DAR evolution showed that the atrazine residence time depends both on the run-off in the first centimetres of the soil and on the treatment periods, particularly in the Grand Morin. The Marne river contamination level was similar to that of the Mélarchez and of the Grand Morin. The minor pollution of the Orgeval was related to minor cultivated areas.

Atrazine↗
PubMed2000

Occurrence and load of selected herbicides and metabolites in the lower Mississippi River.

Analyses of water samples collected from the Mississippi River at Baton Rouge, Louisiana, during 1991-1997 indicate that hundreds of metric tons of herbicides and herbicide metabolites are being discharged annually to the Gulf of Mexico. Atrazine, metolachlor, and the ethane-sulfonic acid metabolite of alachlor (alachlor ESA) were the most frequently detected herbicides and, in general, were present in the largest concentrations. Almost 80% of the annual herbicide load to the Gulf of Mexico occurred during the growing season from May to August. The concentrations and loads of alachlor in the Mississippi River decreased dramatically after 1993 in response to decreased use in the basin. In contrast, the concentrations and loads of acetochlor increased after 1994, reflecting its role as a replacement for alachlor. The peak annual herbicide load occurred in 1993, when approximately 640 metric tons (t) of atrazine, 320 t of cyanazine, 215 t of metolachlor, 53 t of simazine, and 50 t of alachlor were discharged to the Gulf of Mexico. The annual loads of atrazine and cyanazine were generally 1-2% of the amount annually applied in the Mississippi River drainage basin; the annual loads of acetochlor, alachlor, and metolachlor were generally less than 1%. Despite a reduction in atrazine use, historical data do not indicate a long-term downward trend in the atrazine load to the Gulf of Mexico. Although a relation (r2 = 0.62) exists between the atrazine load and stream discharge during May to August, variations in herbicide use and rainfall patterns within subbasins can have a large effect on herbicide loads in the Mississippi River Basin and probably explain a large part of the annual variation in atrazine load to the Gulf of Mexico.

Acetamides↗
PubMedDate not supplied

Rapid screening of triazines and quantitative determination in drinking water.

A sensitive, rapid and inexpensive analysis method has been developed for the triazines most frequently used in Palestine; the method includes fluorodensitometric screening and densitometric determination of the individual substances. Terbutryn as a model substance was derivatized with dansyl chloride in sodium hydrogen-carbonate or phosphate buffer solution to yield a green-blue fluorescent compound. Derivatization occurred at 120 degrees C within maximum of 10-min reaction time. The fluorescent compound formed was separated from excess reagent and other by-products on silica gel TLC plates and was then determined fluorodensitometrically. A linearity range between 20 and 1200 pg/spot was achieved. The method was also applied to other triazine herbicides such as ametryn, atrazine, propazine, terbuthylazine and simazine. Drinking water samples spiked with triazines were extracted using RP-C18 polar plus cartridges, and the extract could be then dansylated as a total. Recoveries were between 88% and 95%; the detection limit was 10 pg/spot and could be further improved to 2 pg/spot by a dipping solution. For quantification, each of the six triazines can be separated on one of three different stationary phases after solid phase extraction and measured densitometrically. The LOD for each individual triazine was 100 ng/l.

Chromatography, Thin Layer↗
PubMed2003

Optical whole-cell biosensor using Chlorella vulgaris designed for monitoring herbicides.

An optical biosensor was designed for determination of herbicides as aquatic contaminants. Detection was obtained with immobilised Chlorella vulgaris microalgae entrapped on a quartz microfibre filter and placed in a five-membrane-home-made-flow cell. The algal chlorophyll fluorescence modified by the presence of herbicides was collected at the tip of an optical fibre bundle and sent to a fluorimeter. A continuous culture was set up to produce algal cells in reproducible conditions for measurement optimisation. Effects of flow rate, algal density, temperature, and pH on the biosensor response to atrazine were studied. Reversibility and detection limits were determined for DNOC and atrazine, simazine, isoproturon, diuron. Detection of photosystem II (PSII) herbicides was achieved at sub-ppb concentration level.

Atrazine↗
PubMed2001

Stable association complex electrospray mass spectrometry for the determination of cyanuric acid.

Cyanuric acid, a suspected gastrointestinal or liver toxicant, has gained interest as a potential degradation product of triazine herbicides, such as simazine and atrazine. This paper investigates the determination of cyanuric acid by stable association complex electrospray mass spectrometry (cESI-MS). The cyanuric acid is extracted from the water through a microscale liquid-liquid extraction. The extract is evaporated to dryness, and an aqueous solution of quaternary ammonium cationic surfactant is added. When injected into the electrospray mass spectrometer, the surfactant and the cyanuric acid form a mass-selective stable association complex, which may be used for confident quantification of cyanuric acid. Several extraction solvents and surfactants were investigated. These studies provide insight into the mechanism of electrospray for the formation of these complexes, specifically with regard to the surface activity of the different surfactants and the chemistry of the surfactant-cyanuric acid complexes. From an analytical standpoint, the cESI-MS method detection limit for extraction of a 1 mL aqueous solution of cyanuric acid was 130 microg/L based on 3.14sigma(n-1) of seven replicate injections. Standard additions were used for quantification of eight aqueous samples. The cyanuric acid concentrations determined with cESI-MS were not significantly different at the 95% confidence level to those determined by conventional high-performance liquid chromatography (HPLC). A recovery of 100% from a fortified urine sample illustrates the robustness of the technique.

Chromatography, High Pressure Liquid↗