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PubMed1992

Comparison of gas chromatographic-mass spectrometric methods for screening of chlorotriazine pesticides in soil.

The performance of a coupled technique resulting from the combination of gas chromatography with a selective mass spectrometric technique (tandem mass spectrometry) (GC-MS-MS) with collisionally activated dissociation (CAD) and multi-reaction monitoring (MRM) was compared with that of GC-low resolution MS (GC-LRMS) at a resolving power of 1000 and GC-high-resolution MS (GC-HRMS) at resolving powers of 5000 and 10,000 for the determination of atrazine, simazine, cyanazine, deethylatrazine and deisopropylatrazine in polluted soil samples. GC-MS-MS daughter ion spectra for the parent ions [M]+. and [M - CH3]+ were generated using collisionally activated dissociation and studied. Also, by optimizing the collision energy for maximum sensitivity a method for screening chlorotriazines by MRM was developed. Analyses of soil sample extracts showed that GC-MS-MS overcomes interferences from other chlorotriazines and interfering compounds that could not be removed by GC-HRMS or GC-LRMS at resolving powers of 10,000 and 1000, respectively. The limits of detection for GC-MS-MS and GC-HRMS at a signal-to-noise ratio of 10 ranged between 1 and 24 pg, with a mean relative standard deviation of 25-30%. Soil samples known to contain chlorotriazines and their degradation products were analysed by GC-MS-MS and the results obtained were compared with those given by GC-HRMS at resolving powers of 5000 and 10,000, with quantification differences of 25-30%.

Gas Chromatography-Mass Spectrometry↗
PubMed1993

Solid-phase extraction followed by high-performance liquid chromatographic analysis for monitoring herbicides in drinking water.

A multiresidue analytical method based on C18 solid-phase extraction and one-run HPLC determination has been developed for the analysis of eleven acidic, neutral and weak basic herbicides in drinking water. A 1-1 sample of water was preconcentrated by passage through a 500-mg C18 solid phase extraction column. The retained compounds were eluted from the column with 1 ml of methanol. After concentration of the extract the pesticides were separated and quantified by reversed-phase HPLC with UV detection. Bentazone, 2,4-D, MCPA, fluazifop-acid, metoxuron, monolinuron, metobromuron, diuron, linuron, atrazine and simazine were determined simultaneously in a single run on a C18 HPLC column. Reanalyses of the sample extracts on a second cyano column were used to confirm the identity of the neutral and basic compounds. The limit of determination, defined as four times the baseline noise, varied between 0.01 microgram/l and 0.1 microgram/l depending on the compound, the detection sensitivity of the instrument and the type of HPLC column used.

Chromatography, High Pressure Liquid↗
PubMed1994

Determination of organophosphorus and triazine pesticides in ground- and drinking water by solid-phase extraction and gas chromatography with nitrogen-phosphorus or mass spectrometric detection.

Trace enrichment and determination of ethoprophos, fenamiphos, fenthion, isophenphos, mevinphos, monocrotophos, atrazine and simazine were performed by solid-phase extraction on XAD-2 columns and Sep-Pak C18 cartridges, subsequent elution with an organic solvent and determination by GC with nitrogen-phosphorus detection (NPD) and mass spectrometry in the selected-ion monitoring mode (MS-SIM). Ground- and drinking water volumes of 1-2.5 l at concentrations levels of 0.1-5 micrograms/l were used for application of the method. Both adsorbents provided recoveries of 75-95%. The limits of detection were 0.08-0.60 micrograms/l with NPD and 0.03-0.13 micrograms/l with MS-SIM.

Gas Chromatography-Mass Spectrometry↗
PubMed1994

Photochemical decomposition of organic compounds in water after UV-irradiation: investigation of positive mutagenic effects.

It should be investigated whether UV-disinfection of natural and contaminated organic substances in surface and drinking water may generate a positive mutagenic effect. Selected organic pesticides (atrazine, simazine, metobromurone, methabenzthiazurone, dichlorprop) and organic compounds naturally present in water (phenylalanine, tyrosine, polysaccharides) were examined in Ames-test (bacterial strains TA 98 and TA 100) and sister chromatid exchange (SCE)-test (V79 cells) before and after UV-irradiation. UV-irradiation with low- and high-pressure mercury vapor lamps was carried out in parallel experiments. Based on results in Ames- and SCE-test a mutagenic activity was not obtained for all samples, neither before nor after UV-irradiation.

Animals↗
PubMed2004

Plasma retinoid profile in bullfrogs, Rana catesbeiana, in relation to agricultural intensity of sub-watersheds in the Yamaska River drainage basin, Québec, Canada.

Amphibian populations are decreasing globally and the causes are presently unclear. Retinoids have been extensively studied in other vertebrate classes where they are associated with pleiotropic effects such as susceptibility to disease (including cancer and parasitic infections), deformities and reproduction. To investigate the hypothesis that retinoid homeostasis is influenced by agricultural activities, blood samples were collected from adult bullfrogs, Rana catesbeiana, at each of six sub-watersheds chosen to represent a gradient of agricultural intensity within the Yamaska River drainage basin. Samples of surface water were collected at each of the study sites approximately 1 month after spraying and analyzed for 53 pesticides. Male body weight was significantly different (p<0.001) between study sites with the smallest bullfrogs captured from the Rivière à la Barbue sub-watershed associated with high agricultural intensity. A significant linear regression (p<0.001; R2=0.176) was obtained between plasma retinol and body weight. Plasma retinol concentrations were significantly different between study sites (p<0.001) being lowest at both Rivière Noire and Rivière à la Barbue. More than 60% of the land area in these sub-watersheds is under intensive corn-soya cultivation and surface water contained the highest concentrations of the herbicides atrazine, deethyl-atrazine, simazine, metolachlor, dimethenamide, chlopyralide, dicamba and bentazone. Plasma 13-cis-4-oxo-retinoic acid was significantly different (p<0.001) between sub-watersheds, however this effect was apparently unrelated to agricultural intensity. Plasma retinol was negatively correlated (p=0.026; r=-0.237) with plasma 13-cis-4-oxo-retinoic acid. These results suggest that retinoid homeostasis in bullfrogs may be influenced by agricultural practices.

Agriculture↗
PubMed2006

Combined effects of herbicides on biomarkers reflecting immune-endocrine interactions in goldfish. Immune and antioxidant effects.

Goldfish (Carassius auratus) were exposed to a mixture of herbicides, namely atrazine, simazine, diuron, and isoproturon (ASDI) at a cumulative concentration of 50microg/l for 12 weeks. Control fish and exposed fish were sampled at 4, 8 and 12 weeks of exposure to observe the combined impact of herbicides on non-specific and specific mechanisms of immunity and antioxidant defenses. The antioxidant defenses were evaluated in haemopoietic organs and liver. ASDI-induced stress was reflected as a significant induction of superoxide (O(2)(-)) production in phagocytic cells of head kidney and spleen. In addition, plasma lysozyme activity was consistently high in the treatment group. Specific immunity was assessed by antibody titre responses following immunization of the fish with sheep red blood cells (SRBCs). Antibody titre was reduced throughout the period of observation in ASDI-treated fish. This reduction was found to be significant at week 4 (p<0.05). Herbicide-exposed fish showed reduced resistance against pathogen invasion but remarkable enhancement in lysozyme activity. The ASDI-induced oxidative stress in spleen, kidney and liver was reflected as a change in the antioxidant enzyme activities in these vital organs of fish. Our data indicate that herbicides at concentrations present in water bodies in Europe cause immune suppression in goldfish.

Aeromonas hydrophila↗
PubMed2004

Isolation of a member of Acinetobacter species involved in atrazine degradation.

Contribution of Acinetobacter genus in the degradation of atrazine and its analogs is reported here. An interesting bacterial isolate capable of degrading atrazine as high as 250 ppm was isolated from a soil heavily contaminated with atrazine. The permissible level of atrazine in drinking water is 3 ppb and hence use of a strain capable of atrazine degradation as high as 250 ppm would be of immense help for rapid environmental cleanup. This isolate was found to be capable of best growth at 37 degrees C and at pH inclined towards the alkaline side. It was found that atrazine was utilized as a carbon and not as a nitrogen source. Acinetobacter species was also active on other triazine pesticides, viz., simazine, terbutryn, cyanazine, and prometon. There are very few reports on the degradation of atrazine by any member of this genus and hence this could lead to new degradation pathways and new metabolites.

Acinetobacter↗
PubMed2005

Phytotoxicity of surface waters of the Thames and Brisbane River estuaries: a combined chemical analysis and bioassay approach for the comparison of two systems.

The Thames Estuary, UK, and the Brisbane River, Australia, are comparable in size and catchment area. Both are representative of the large and growing number of the world's estuaries associated with major cities. Principle differences between the two systems relate to climate and human population pressures. In order to assess the potential phytotoxic impact of herbicide residues in the estuaries, surface waters were analysed with a PAM fluorometry-based bioassay that employs the photosynthetic efficiency (photosystem II quantum yield) of laboratory cultured microalgae, as an endpoint measure of phytotoxicity. In addition, surface waters were chemically analysed for a limited number of herbicides. Diuron, atrazine and simazine were detected in both systems at comparable concentrations. In contrast, bioassay results revealed that whilst detected herbicides accounted for the observed phytotoxicity of Brisbane River extracts with great accuracy, they consistently explained only around 50% of the phytotoxicity induced by Thames Estuary extracts. Unaccounted for phytotoxicity in Thames surface waters is indicative of unidentified phytotoxins. The greatest phytotoxic response was measured at Charing Cross, Thames Estuary, and corresponded to a diuron equivalent concentration of 180 ng L(-1). The study employs relative potencies (REP) of PSII impacting herbicides and demonstrates that chemical analysis alone is prone to omission of valuable information. Results of the study provide support for the incorporation of bioassays into routine monitoring programs where bioassay data may be used to predict and verify chemical contamination data, alert to unidentified compounds and provide the user with information regarding cumulative toxicity of complex mixtures.

Australia↗
PubMed2006

Study of the presence of pesticides in surface waters in the Ebro river basin (Spain).

This work studies the presence of a total number of 44 substances found in waters of the Ebro river basin (Spain), all included in the Pesticides Control Network, whose purpose is to monitor diffuse pollution of surface waters caused by pesticides contained in some of the dangerous substances lists established in existing legislation and their high degree of use in the basin. Most of the pesticide sampling points are located in the sections of river that receive run-off waters from various agricultural areas shortly before opening out onto the main river (the Ebro), in areas of special agricultural importance. Water samples are subjected to a solid-liquid extraction as a previous step to their analysis by GC/MS (gas chromatography/mass spectrometry). Pesticides most frequently found and in greater concentrations in the waters of the Ebro river basin are 3,4-dichloroaniline, molinate, desethylatrazine, dimetoate, simazine, atrazine, metolachlor and chlorpyrifos. There are certain compounds that are not detected or their concentrations are below the quantification limit, such as 4-isopropylaniline, ametryn, beta-HCH, delta-HCH, aldrin, isodrin, dieldrin, heptachlor epoxide, endosulfan and endosulfan-sulfate. Diuron appears at specific points in some of the stations.

Environmental Monitoring↗
PubMed2006

Organic contaminant loads into the Western Mediterranean Sea: estimate of Ebro River inputs.

Annual input estimates for several organic contaminants from the Ebro River into the Northwestern Mediterranean Sea were carried out on the basis of monthly sampling from November 2002 to October 2003. Some organochlorine compounds (DDT and its degradation products, DDD and DDE, PCBs (9 congeners), HCB and gamma-HCH) were selected due to their reported occurrence in the river. Furthermore, some polar pesticides used in the Ebro Delta were also determined (atrazine, simazine, diazinon, fenitrothion and molinate). Concentrations ranged from 0.4 to 19.5 ng l(-1) for the organochlorine compounds (sum of particulate and dissolved phases) and from not detected (ND) to 170 ng l(-1) for the more polar pesticides, which were only found in the dissolved phase. The sum of PCB congeners (mean 8.9 ng l(-1)) showed the highest concentrations among the organochlorine compounds and atrazine (mean 82 ng l(-1)) among the polar pesticides. Based on the contaminant concentrations and on hydrological data, contaminant discharges into the sea were estimated amounting in total to 167 and 1,258 kg year(-1) of organochlorine compounds and polar pesticides, respectively. Furthermore, it was observed that PCBs, DDTs and HCB inputs were basically influenced by spate periods due to an increase in suspended particulate matter associated to runoff and sediment resuspension. Whereas for more water soluble contaminants, such as the agrochemicals, their seasonal use had a higher incidence in contaminant fluxes. Bulk chemical parameters such as SPM, DOC, POC, %OC, %ON and C/N ratio provided additional information on the organic matter sources. This provides a better understanding of the temporal variability of the contaminant concentrations.

Animals↗
PubMed2004

New materials for solid-phase extraction and multiclass high-performance liquid chromatographic analysis of pesticides in grapes.

Sample preparation procedures which included the use of new aminopropyl (NH2) and octadecyl (C18) solid-phase extraction (SPE) sorbents are proposed for the simultaneous multiclass determination of the fungicide benomyl and of the herbicides tebuthiuron, diuron, simazine, atrazine, and ametryn in grapes, using single wavelength high-performance liquid chromatography. Sorbent preparation uses a fast, easy, and effective procedure to obtain silica-based materials, made by depositing polysiloxanes on a silica support followed by thermal immobilization. Recovery results of the compounds, after elution from the SPE cartridges, indicate that the most efficient system employed silica loaded with 40% of an aminofunctional polydimethylsiloxane as sorbent, using dichloromethane:methanol (95:5, v/v) as eluent. Method validation, carried out in agreement with International Conference on Harmonization directives, was performed at three fortification levels (100, 200, and 1000 microg kg(-1)). Limits of detection and quantification show that the method developed can be used to detect the pesticides at concentrations below the maximum residue levels established by Codex Alimentarius, the US Environmental Protection Agency, the European Union, and Brazilian legislation.

Chromatography, High Pressure Liquid↗
PubMed2005

High-performance liquid chromatographic determination of pesticides in tomatoes using laboratory-made NH2 and C18 solid-phase extraction materials.

A method for high-performance liquid chromatographic (HPLC) multiresidue determination of six pesticides in tomatoes was developed and validated. Silica-based C18 (octadecyl) and NH2 (aminopropyl) solid-phase extraction (SPE) sorbents, made in our laboratory, were used for sample preparation. The SPE materials were obtained by thermal immobilization of appropriate polysiloxanes onto 40 microm silica surfaces and were used in sample preparation for multiresidue analysis of the following pesticides: tebuthiuron and diuron (urea herbicides), simazine, atrazine and ametryn (triazines herbicides) and benomyl (benzimidazol fungicide). The results were compared with similar commercial materials. Reversed-phase high-performance liquid chromatography (RP-HPLC) using a Purospher RP-18 5 microm column and ACN: 0.01% aqueous NH4OH, pH 8.4 (35:65, v/v) as mobile phase, at 0.7 mlmin(-1), with 235 nm UV detection, was used for separation and quantification of the pesticides. Method validation was performed at three fortification levels (100, 200, 1000 microg l(-1)). Limits of detection and quantification show that the methods developed can be used to detect the pesticides in concentrations below the maximum residue levels (MRL) established by the Codex Alimentarius, USA, European Union and Brazilian legislations. The results showed that aminopropyl materials have a better performance than the octadecyl sorbents. Laboratory-made materials give results similar to commercial sorbents, with recoveries and precisions in agreement with directives for method validation in residue analysis.

Chromatography, High Pressure Liquid↗
PubMed2005

Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry.

A novel analytical approach has been developed and evaluated for the quantitative analysis of a selected group of widely used pesticides (dimethoate, simazine, atrazine, diuron, terbuthylazine, methyl-parathion, methyl-pirimiphos, endosulfan I, endosulfan II, endosulfan sulphate, cypermethrin and deltamethrin), which can be found at trace levels in olive oil and olives. The proposed methodology is based on matrix solid-phase dispersion (MSPD), (with a preliminary liquid-liquid extraction in olive oil samples) using aminopropyl as sorbent material with a clean-up performed in the elution step with Florisil, followed by mass spectrometric identification and quantitation of the selected pesticides using both gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode and liquid chromatography tandem mass spectrometry (LC-MS-MS) in positive ionization mode. The recoveries obtained (with mean values between 85 and 115% (obtained at different fortification levels) with RSD values below 10% in most cases, confirm the usefulness of the proposed methodology for the analyses of these kind of complex samples with a high fat content. Moreover, the obtained detection limits, which were below 5 microg kg(-1) by LC-MS analyses and ranged from 10 to 60 microg kg(-1) by GC-MS meet the requirements established by the olive oil pesticide regulatory programs. The method was satisfactorily applied to different olives and olive oil samples.

Dimethoate↗
PubMed2006

On-fibre solid-phase microextraction coupled to conventional liquid chromatography versus in-tube solid-phase microextraction coupled to capillary liquid chromatography for the screening analysis of triazines in water samples.

This paper compares the advantages and disadvantages of two different configurations for the extraction of triazines from water samples: (1) on-fibre solid-phase microextraction (SPME) coupled to conventional liquid chromatography (LC); and (2) in-tube SPME coupled to capillary LC. In-tube SPME has been effected either with a packed column or with an open capillary column. A critical evaluation of the main parameters affecting the performance of each method has been carried out in order to select the most suitable approach according to the requirements of the analysis. In the on-fibre SPME configuration the fibre coating was polydimethylsiloxane (PDMS)-divinylbenzene (DVB). The limits of detection (LODs) obtained with this approach under the optimized extraction and desorption conditions were between 25 and 125 microg/L. The in-tube SPME approach with a C18 packed column (35 mm x 0.5 mm I.D., 5 microm particle size) connected to a switching micro-valve provided the best sensitivity; under such configuration the LODs were between 0.025 and 0.5 microg/L. The in-tube SPME approach with an open capillary column coated with PDMS (30 cm x 0.25 mm I.D., 0.25 microm of thickness coating) connected to the injection valve provided LODs between 0.1 and 0.5 microg/L. In all configurations UV detection at 230 nm was used. Atrazine, simazine, propazine, ametryn, prometryn and terbutryn were selected as model compounds.

Chromatography, Liquid↗
PubMed2006

Toxicity assessment of 40 herbicides to the green alga Raphidocelis subcapitata.

The effects of 40 herbicides with nine modes of action on the green alga Raphidocelis subcapitata were studied by 96-h acute toxicity tests. Results showed that the EC50 of the herbicides with respect to the photosynthetic processes of R. subcapitata ranged from 0.0007 to 4.2286 mgL(-1). Photosynthesis was the process of the green alga most sensitive to the tested herbicides. The most toxic herbicides were atrazine, ametryme, simazine, prometryne, cyanazine, isoproturon, chlorotoluron, diuron, methabenzthiazuron, and paraquat. The EC50 of the protoporphyrinogen oxidase inhibitor oxadiargyl, which was the parameter least sensitive to the herbicides tested in this study, was 42.5 mgL(-1). The descending order of the average acute toxicity to R. subcapitata of herbicides with regard to the nine modes of action was as follows: photosynthetic process>cell division>lipid synthesis, acetyl-coenzyme A carboxylase>acetolactate synthase> 5-enolpyruvyl-shikimate-3-phosphate synthase, glutamine synthase, hormone synthesis>protoporphyrinogen oxidase.

Chlorophyta↗
PubMed2005

Seasonal exposures to triazine and other pesticides in surface waters in the western Highveld corn-production region in South Africa.

The objective of this study was to characterize concentrations of atrazine, terbuthylazine, and other pesticides in amphibian habitats in surface waters of a corn-production area of the western Highveld region (North-West Province) of South Africa. The study was conducted from November 2001 to June 2002, coinciding with the corn-production season. Pesticide residues were measured at regular intervals in surface water from eight ponds, three in a non-corn-growing area (NCGA) and five within the corn-growing area (CGA). Measured atrazine concentrations differed significantly among sites and between samples. In the five CGA sites, the maximum atrazine concentrations measured during the study ranged from 1.2 to 9.3 microg/L. Although no atrazine was recorded as being applied in the catchment of the three NCGA sites, maximum concentrations from 0.39 to 0.84 microg/L were measured during the study, possibly as a result of atmospheric transport. Maximum measured concentrations of terbuthylazine ranged from 1.22 to 2.1 microg/L in the NCGA sites and from 1.04 to 4.1 microg/L in the CGA sites. The source of terbuthylazine in the NCGA sites may have been in use other than in corn. The triazine degradation products, deisopropylatrazine (DIA) and deethylatrazine (DEA) and diaminochlorotriazine (DACT) were also found in water from both the CGA and NCGA sites. Concentrations of DIA were > or = 1 microg/L throughout the season, while DEA concentrations were mostly <0.5 microg/L before planting but increased after planting and application of herbicides to concentrations >2 microg/L in some locations. Concentrations of DACT were highly variable (LOD to 8 microg/L) both before and after planting and application, suggesting that they resulted from historical use of triazines in the area. Other herbicides such as simazine and acetochlor were only detected infrequently and pesticides such as S-metolachlor, cypermethrin, monocrotophos, and terbuphos, known to be used in the CGA, were not detected in any of the samples. Because of dilution by higher than normal rainfall in the study period, these concentrations may not be predictive of those in years of normal rainfall.

Agriculture↗
PubMed2005

The status of pesticide pollution in surface waters (rivers and lakes) of Greece. Part I. Review on occurrence and levels.

This review evaluates and summarizes the results of long-term research projects, monitoring programs and published papers concerning the pollution of surface waters (rivers and lakes) of Greece by pesticides. Pesticide classes mostly detected involve herbicides used extensively in corn, cotton and rice production, organophosphorus insecticides as well as the banned organochlorines insecticides due to their persistence in the aquatic environment. The compounds most frequently detected were atrazine, simazine, alachlor, metolachlor and trifluralin of the herbicides, diazinon, parathion methyl of the insecticides and lindane, endosulfan and aldrin of the organochlorine pesticides. Rivers were found to be more polluted than lakes. The detected concentrations of most pesticides follow a seasonal variation, with maximum values occurring during the late spring and summer period followed by a decrease during winter. Nationwide, in many cases the reported concentrations ranged in low ppb levels. However, elevated concentrations were recorded in areas of high pesticide use and intense agricultural practices. Generally, similar trends and levels of pesticides were found in Greek rivers compared to pesticide contamination in other European rivers. Monitoring of the Greek water resources for pesticide residues must continue, especially in agricultural regions, because the nationwide patterns of pesticide use are constantly changing. Moreover, emphasis should be placed on degradation products not sufficiently studied so far.

Agriculture↗
PubMed2004

Characterisation and quality assessment of binding sites on a propazine-imprinted polymer prepared by precipitation polymerisation.

In this paper, the Langmuir-Freundlich isotherm (LF) is used to characterise a propazine-imprinted polymer obtained by precipitation polymerisation (MIP-P). Different rebinding studies were carried out allowing to explain the different interactions taking place between the molecularly imprinted polymer and six triazinic herbicides (desisopropylatrazine, desethylatrazine, simazine, atrazine, propazine and prometryn). The LF fitting parameters obtained (total number of binding sites, heterogeneity index and mean binding affinity) were compared to those obtained in a previous work for a propazine-imprinted polymer prepared by bulk polymerisation (MIP-B). From that study, it was concluded that precipitation polymerisation yielded polymers with a more homogeneous binding site distribution and higher affinity constants.

Binding Sites↗