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1.
A commercial magnetic particle-based enzyme-linked immunosorbent assay (ELISA) kit for the insecticide chlorpyrifos [O,O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate] was evaluated for its specificity, precision, and accuracy, its susceptibility to matrix interferences in agricultural and environmental surface waters, and its comparability to a gas chromatographic/flame photometric (GC/FPD) method for the determination of organophosphorus pesticides in natural waters. Repeatability, reproducibility, and accuracy studies show that the kit satisfies current U.S. Environmental Protection Agency criteria for the assessment of analytical methods. Observable matrix effects were found to be present in all of the environmental test waters, with the slopes of calibration curves generated in each of the test matrices deviating from that of the control matrix by as much as 16%. Specificity studies indicate that the chlorpyrifos polyclonal antibody adequately differentiates the target compound from other structurally similar organophosphorus pesticides, with the exception of its methyl analogue. Cross-reactivity with chlorpyrifos-methyl was approximately 37%, while reactivity with diazinon, pyridaphenthion, diclofenthion, bromiphos-ethyl, bromiphos-methyl, pirimiphos-ethyl, and chlorpyrifos oxon ranged from 1.6 to 10.7%. Cross-reactivity with pirimiphos-methyl, 3,5,6-trichloro-2-pyridinol, diethyl phosphate, and diethyl thiophosphate was negligible (<1%). Validation of the paramagnetic particle ELISA format was accomplished using water samples from two monitoring studies that were collected, split, and analyzed directly by ELISA and by GC/FPD. Results of the two analytical methods were then compared using standard t tests, regression analysis, and differences against mean measurement (bias) plots. While the agreement between the two methods was determined to be satisfactory, ELISA exhibits consistent positive bias in environmental matrices. Several preanalysis mitigation steps were suggested that may help moderate bias, but additional study is recommended to explicate the exact factors responsible for its consistent overestimation of results.  相似文献   

2.
The performance of a commercially available microtiter plate ELISA kit for the determination of the neonicotinoid insecticide imidacloprid was evaluated for sensitivity, selectivity, influence of organic solvent used for extraction procedure, matrix interference originated from agricultural sample, accuracy, and method comparison with conventional HPLC analysis. The limit of detection for the kit (0.1 or 0.5 ng/mL) was determined. The working range (1-39 ng/mL) experimentally calculated on the basis of a criterion, which is determined as the range from I(20) to I(80), was comparable to that established by the manufacturer (1-50 ng/mL). The linearity of the standard curve based on the kit-assembled standard solutions agreed with the one based on the self-made standard solutions. Specificity studies indicate that the imidacloprid monoclonal antibody can readily distinguish the target compound from other structurally related neonicotinoid analogues and some metabolites, with the exception of clothianidin, the cross-reactivity of which was approximately 12%. To extract imidacloprid from an agricultural sample (apple) as simply and rapidly as possible, some extraction methods were examined. Consequently, the extraction method with hand-shaking for 5 min was the best among the examined methods. For the analysis of imidacloprid in apple samples, it was extracted directly with methanol and the extracts were diluted 10-fold (100-fold in the well) with water prior to ELISA analysis. No significant matrix interference was observed with the dilution factor. Recoveries of imidacloprid from fortified apple samples ranged from 87.7 to 112.0%. The results obtained with the ELISA kit correlated well with those by the reference method (conventional HPLC analysis) for apple samples (r > 0.998). These findings strongly indicate that the ELISA kit may be employed routinely for an on-site imidacloprid residue analysis of apple samples.  相似文献   

3.
In previous studies, polyclonal antibodies against the organophosphorus insecticide fenthion were obtained and an indirect competitive enzyme-linked immunosorbent assay (ELISA) was developed for this pesticide. In this study, using these antibodies and an enzyme tracer, direct competitive ELISAs for fenthion in microtiter plate and dipstick formats were developed. The microtiter plate ELISA showed an IC(50) value of 1.2 microg/L with a detection limit of 0.1 microg/L. The antibodies showed negligible cross-reactivity with other organophosphorus pesticides. The use of the dipstick format using Immunodyne as a support membrane allowed the quick visual detection of fenthion in concentrations >10 microg/L. The IC(50) value of the dipstick format using reflectance detection was 15 microg/L with a detection limit of 0.5 microg/L. The recoveries of fenthion from spiked vegetable samples using the two formats without any prior enrichment or cleanup steps were 87-116%.  相似文献   

4.
Diazinon Mitigation in Constructed Wetlands: Influence of Vegetation   总被引：1，自引：0，他引：1  
In intensively cultivated areas, agriculture is a significant source of pesticides associated with storm runoff. When these pollutants enter aquatic receiving waters, they have potential to damage nearby aquatic ecosystems. Constructed wetlands are a best management practice (BMP) designed to help alleviate this potential problem. A constructed wetland system (180?×?30 m) comprised of a sediment retention basin and two treatment cells was used to determine fate and transport of a simulated storm runoff event containing the insecticide diazinon and suspended sediment. Wetland water, sediment, and plant samples were collected spatially and temporally over 55 d. Results indicated that 43% of the study’s measured diazinon mass was associated with plant material, while 23 and 34% were measured in sediment and water, respectively. Mean diazinon concentrations in water, sediment, and plants for the 55-d study were 18.1?±?4.5 μg/l, 26.0?±?8.0 μg/kg, and 97.8?±?10.7 μg/kg, respectively. Aqueous concentrations fluctuated in the wetlands between 51–86 μg/l for the first 4 h of the experiment; however, by 9 h, aqueous concentrations were approximately 16 μg/l. During the 55 d experiment, 0.3 m of rainfall contributed to fluctuations in diazinon concentrations. Results of this experiment can be used to model future design specifications for mitigation of diazinon and other pesticides.  相似文献   

5.
Naturally contaminated corn and cottonseed samples were screened for aflatoxin B1 (AFB1) by a direct competitive enzyme-linked immunosorbent assay (ELISA). Samples were blended 5 min in an extraction solvent of methanol-water-dimethylformamide (70 + 29 + 1) and filtered. Filtrates were assayed by direct competition between AFB1 in the corn and cottonseed samples and AFB1-peroxidase conjugate for binding to specific antibody adsorbed to a solid phase microtiter plate. Standard curves prepared using the extract of AFB1-free corn and cottonseed samples, and extraction solvent only, showed negligible interference by the sample extract in the performance of ELISA. The AFB1 content in corn and dehulled cottonseed samples as determined by ELISA ranged from 7 to 422 micrograms/kg and 7 to 3,258 micrograms/kg, respectively. When ELISA estimates of AFB1 in corn were compared with values obtained by thin layer chromatography (CB method), the correlation coefficient (n = 10) was 0.95. Average interassay and subsample coefficients of variation for ELISA in corn were 21.4 and 22.0%, respectively. When ELISA estimates of AFB1 in cottonseed were compared with values obtained by liquid chromatography (Pons method), the correlation coefficient (n = 15) was 0.96. Using this ELISA, 36 duplicate sample extracts can be screened for AFB1 in less than 2 h.  相似文献   

6.
Investigations of agricultural nonpoint source pollution typically focus on a relatively narrow range of targeted toxic and biostimulatory compounds (e.g., specific pesticides, nutrients). Regular application of numerous other organic compounds to agricultural fields in pesticide formulations, irrigation water, soil amendments, and fertilizers may result in their transport into surface waters via runoff. We examined whether potentially toxic dissolved and particle-associated "nontarget" organic compounds were present in surface runoff from agricultural fields irrigated with disinfected tertiary recycled water or wastewater effluent-dominated streamwater. Gas chromatographic-mass spectrometric analyses of filtered runoff samples revealed the presence of numerous nontarget compounds of potential toxicological significance including pesticide transformation products, pesticide adjuvant chemicals, plasticizers, flame retardants, pharmaceuticals, and personal care product ingredients. Although the toxicity of many of these compounds is poorly characterized, some may elicit subtle but profound toxicological effects. Agricultural runoff also represented a source of allochthonous natural organic matter to the stream system.  相似文献   

7.
Recycling or collection ponds are often used in outdoor container nursery production to capture and recycle runoff water and fertilizers. Waters in recycling ponds generally have high concentrations of nutrients, pesticides, and dissolved organic matter, as well as elevated salinity and turbidity. Little is known about pesticide degradation behavior in the unique environment of nursery recycling ponds. In this study, degradation of four commonly used pesticides diazinon, chlorpyrifos, chlorothalonil, and pendimethalin in waters from two nursery recycling ponds was investigated at an initial pesticide concentration of 50 microg/L. Results showed that the persistence of diazinon and chlorpyrifos appeared to be prolonged in recycling pond waters as compared to surface streamwaters, possibly due to decreased contribution from biotic transformation, while degradation of chlorothalonil and pendimethalin was enhanced. Activation energies of biotic degradation of all four pesticides were lower than abiotic degradation, indicating that microbial transformation was less affected by temperature than chemical transformation. Overall, the pesticide degradation capacity of recycling ponds was better buffered against temperature changes than that of surface streamwaters.  相似文献   

8.
A competitive enzyme-linked immunoassay (ELISA) for the quantitation of Penoxsulam [2-(2,2-difluoroethoxy)-6-(trifluoromethyl-N-(5,8-dimethoxy[1,2,4]triazolo[1,5-c]pyrimidin-2-yl))benzenesulfonamide] in ground and surface waters was developed. This immunoassay utilizes magnetic particles as the solid phase to which polyclonal rabbit anti-Penoxsulam antibodies are attached. The ELISA has an estimated detection limit of 0.17 ppb (microg/mL) of Penoxsulam in water. Specificity studies indicate that the antibody can distinguish Penoxsulam from its major metabolites and structurally similar pesticides. Interference studies indicate that the ELISA has a wide tolerance of sample pH and salinity and for compounds commonly found in surface and ground waters. The ELISA was shown to compare favorably to LC-MS/MS on ground and surface water samples (r(2) = 0.957). The various studies performed demonstrate the usefulness of the ELISA technique as a rapid and high-throughput analytical method for the cost-effective monitoring of water samples.  相似文献   

9.
Two competitive immunoassays, a laboratory assay based on microwell plates and a field test based on the use of polystyrene tubes, have been developed for the detection of endosulfan in agricultural products. The limit of detection for the microwell plate format was 0.8 +/- 0.1 microg/kg, and the limit of detection for the tube format was 1.6 +/- 0.2 microg/kg. A simple, rapid, and efficient extraction method was employed, and 76-112% recoveries of spiked samples were obtained. Methanol extracts of some agricultural product samples such as grape, carrot, spinach, and tobacco could be analyzed directly by immunoassay after dilution in 0.5% fish skin gelatin-phosphate buffered saline. In contrast, extracts of green tea caused significant interference in the assay, and a number of simple cleanup methods were ineffective in removing interference. However, use of the coagulating reagent polyvinyl pyrrolidone removed the matrix effect effectively. For the validation of the enzyme-linked immunosorbent assay (ELISA) tests, samples were analyzed by ELISA and gas chromatography (GC) after solid phase extraction. The relationship between data obtained using the tube assay and microwell assay was good (the lowest r(2) value was 0.94), and also, the immunoassay assay data correlated well with data obtained from GC analysis (the lowest r(2) value was 0.93). The developed immunoassay methods are the suitable methods for the rapid quantitative and reliable determination of endosulfan residues in agricultural products.  相似文献   

10.
Solid phase microextraction (SPME) is an ideal sample preparation technique because of its speed and solvent-free features. Sampling by SPME is selective and only the dissolved concentration is measured, which allows measurement of the bioavailable fraction of a contaminant in aqueous media. One potential application of SPME is for analysis of enantiomers of chiral contaminants in environmental samples. In this study, a method was developed for determining enantiomers of (Z)-cis-bifenthrin and cis-permethrin in water using coupled SPME and enantioselective gas chromatography (GC). Following SPME sampling, enantiomers of (Z)-cis-bifenthrin and cis-permethrin were separated at the baseline on a beta-cyclodextrin-based enantioselective column, and analyte enrichment onto the SPME fiber was not enantioselective. The GC response increased as sampling time was increased from 0 to 240 min, and as sampling temperature was increased from 20 to 40 degrees C. Organic solvents such as methanol, acetone, and acetonitrile enhanced, while soil extracts slightly decreased, the GC response. The integrated SPME-enantioselective GC method was used to analyze surface runoff samples. The analysis showed preferential degradation of the 1S-3S enantiomer over the 1R-3R enantiomer for both (Z)-cis-bifenthrin and cis-permethrin. The concentrations detected by SPME-GC were substantially smaller than those determined following solvent extraction, suggesting that SPME-enantioselective GC analysis selectively measured the dissolved fraction.  相似文献   

11.
Land development has caused runoff of red soil into the ocean on the north side of Okinawa Island, Japan. In an attempt to clarify the impacts of this “red soil pollution” on the oxidizing power of seawater, we studied the formation of hydroxyl radical (?OH), the most potent oxidant in the environment, in red soil-polluted waters using a 313-nm monochromatic light. ?OH was photochemically formed in the red soil-polluted water samples, and the formation rates of ?OH decreased as salinity increased, i.e., as red soil-polluted river water gets mixed with seawater. The photo-formation rates of ?OH showed good correlations with dissolved Fe concentrations (R 2?=?0.96) and [NO2 ?]?+?[NO3 ?] concentrations (R 2?=?0.87), while a negative and weak correlation was found with dissolved organic carbon concentrations (R?=??0.78). Theoretical calculation showed that direct photolysis of NO3 ?, Fe(OH)2+, and hydrogen peroxide all together accounted for less than 10% of the observed ?OH formation in the red soil-polluted waters. Comparison between filtered and unfiltered samples showed that red soil particles were not the main sources of ?OH, and the photolysis of NO2 ? could account for at most 78% of the observed ?OH formation rates. We found that the Fenton’s reaction (a reaction between Fe(II) and H2O2) could possibly account for the observed formation of ?OH in the red soil-polluted waters.  相似文献   

12.
Examination of naturally occurring C. parvum oocysts from environmental water samples has previously been hampered by the inability to determine the public health significance of detected organisms. As a result the safety of drinking water supplies was in question. These limitations have been resolved through the development and application of a method that incorporates immunomagnetic separation (IMS) and an infectivity determination using an integrated cell culture, polymerase chain reaction assay (CC-PCR). Briefly, the method concentrates water samples by filtration or centrifugation and isolates oocysts by IMS. An acidified Hank's balanced salt solution (HBSS) containing 1% trypsin was used for the dissociation of captured oocysts from the IMS beads. In vitro HCT-8 cell culture of purified oocysts was performed in 96-well microtiter plates and infected cells were detected using PCR primers specific for C. parvum. A total of 242 raw source waters or filter backwash water samples from twenty five sites in the U.S. were analyzed to validate the procedure. Oocyst seeded in raw and filter backwash water samples were used to evaluate recovery efficiencies and performance of the CC-PCR protocol with different water quality matrices. The CC-PCR detected infectious Cryptosporidium parvum in 6 of 121 (5.0%) raw and 9 of 122 (7.4%) filter backwash water samples. All CC-PCR positive samples were confirmed by cloning and DNA sequence analysis of the PCR products. Isolates were shown to originate from human and animal sources. Grouping of genotypes permitted evaluation of strain diversification and variation. Current studies are using this technique to examine oocysts in various watersheds and in the finished drinking water of over 80 surface water treatment plants.  相似文献   

13.
Road runoff waters are able to convey a number of organic and inorganic pollutants originated by different non-point sources and by the road surface itself. Such pollutants can enter aquatic systems, thus contributing to water and soil contamination. This study was aimed at evaluating the pollutant content in first flush runoff waters from a highway located in Central Italy. A water sampling apparatus was devised able to collect only the first 10 L of runoff water. Water samples were analyzed by atomic absorption spectroscopy, ion chromatography, and gas chromatography-mass spectrometry in order to determine metals, ions, and polynuclear aromatic hydrocarbons, respectively. Soil samples were collected as well for metal and hydrocarbon determination. Results obtained in a field experiment carried out in two different seasons and in two different sites along the highway are reported. The study was extended to water samples collected in a strip of the same road not yet in use. Results obtained showed a temporal and a spatial variability due to the different period rainfall and to sites features, respectively. Within such a variability, a substantial agreement, in terms of order of magnitude, with other studies carried out in European sites was observed.  相似文献   

14.
Sorption and degradation are the primary processes controlling the efficacy and runoff contamination risk of agrochemicals. Considering the longevity of biochar in agroecosystems, biochar soil amendment must be carefully evaluated on the basis of the target agrochemical and soil types to achieve agricultural (minimum impact on efficacy) and environmental (minimum runoff contamination) benefits. In this study, sorption-desorption isotherms and kinetics of triazine (deisopropylatrazine) and organophosphorus (malathion, parathion, and diazinon) pesticides were first investigated on various soil types ranging from clayey, acidic Puerto Rican forest soil (PR) to heavy metal contaminated small arms range (SAR) soils of sandy and peaty nature. On PR, malathion sorption did not reach equilibrium during the 3 week study. Comparison of solution-phase molar phosphorus and agrochemical concentrations suggested that degradation products of organophosphorus pesticides were bound on soil surfaces. The degree of sorption on different soils showed the following increasing trend: deisopropylatrazine < malathion < diazinon < parathion. While sorption of deisopropylatrazine on SAR soils was not affected by diazinon or malathion, deisopropylatrazine suppressed the sorption of diazinon and malathion. Deisopropylatrazine irreversibly sorbed on biochars, and greater sorption was observed with higher Brunauer-Emmett-Teller surface area of biochar (4.7-2061 mg g(-1)). The results suggested the utility of biochar for remediation of sites where concentrations of highly stable and mobile agrochemicals exceed the water-quality benchmarks.  相似文献   

15.
施肥深度和用量对华南果园土壤氮磷流失的影响   总被引：9，自引：0，他引：9  
Fertilizers are heavily applied in orchards of the hilly and mountainous topography of South China and may increase nutrient loadings to receiving waters. A simple runoff collecting system was used to measure the effects of different fertilization treatments on total N and P concentrations of surface runoff in a Chinese chestnut （Castanea mollissima Blume） orchard in Dongyuan County, Guangdong Province, China. In such orchards, fertilizer was typically applied in two short furrows or pits on either side of each tree. Treatments included three application depths （surface, 10 cm and 20 cm）, and three application rates （low, median and high）. Results showed that 90.5% of the runoff water samples had a total N concentration higher than 0.35 mg·L^-1 and 54.2% had a total P concentration higher than 0.1 mg·L^-1. Fertilizer application at all depths and at all but the lowest rate significantly increased total N and P concentrations in runoff water. Fertilization with chemical compound fertilizer at a soil depth of 20 cm produced significantly lower （P 〈 0.05） total N concentration in runoff than both surface and 10-cm depth fertilization, and significantly lower （P 〈 0.05） total P concentration in runoff than surface fertilization. Total N and P concentrations in runoff significantly increased with the application rate of organic fertilizers. With the exception of total P concentrations, which were not significantly different between the control and fertilization at a rate of 119 kg P ha-1 in organic form, all the other fertilization treatments produced significantly higher total N and total P concentrations in runoff than the control. A fertilization depth ≥ 20 cm and an application rate ≤ 72 kg N ha-1 or 119 kg P ha^-1 for compound organic fertilizer was suggested to substantially reduce N and P runoff losses from hillslope orchards and to protect receiving waters in South China.  相似文献   

16.
蔬菜地土壤磷饱和度及其对磷释放和水质的影响   总被引：24，自引：0，他引：24  
为了解蔬菜地土壤磷素的积累对水环境的影响,我们在浙江省选择了33个代表性蔬菜地,采集和分析了土壤、地表水和地下水样的磷素状况,从土壤磷饱和度的角度,研究了浙江省主要蔬菜土壤磷积累状况及其对地表和地下水水质和土壤磷释放潜力的影响。结果表明,半透膜渗析法测得的磷释放量与土壤磷积累呈正相关,磷释放量随土壤磷饱和度的提高而增加。蔬菜地土壤磷饱和度的增加可显著提高地表水体和地下水中磷的浓度,当土壤磷饱和度小于25%左右时,水体中磷浓度随土壤磷饱和度增加较为缓慢;但当磷饱和度大于25%时,水体中磷浓度随土壤磷饱和度提高迅速上升。地表水中磷浓度主要与表层土壤磷饱和度有关;地下水中磷浓度主要受深层土壤磷饱和度的影响,与表层土壤磷饱和度的相关性较小。土壤磷饱和度可很好地表征土壤磷释放和对环境的潜在影响。  相似文献   

17.
Irrigation of crops with treated wastewater has the potential to introduce effluent-derived organic microcontaminants into surface waters through agricultural runoff. To determine whether compounds indicative of the presence of treated effluent in irrigation water could be identified in agricultural runoff, surface runoff samples collected from effluent-irrigated and rain-fed cultivated fields were analyzed for a broad spectrum of organic compounds. A variety of compounds was identified that appeared to be associated with irrigation with treated wastewater. These compounds included human pharmaceuticals (e.g., carbamazepine, gemfibrozil, carisoprodol), personal care product ingredients (e.g., insect repellent, polycyclic musks), and alkyl phosphate flame retardant chemicals. Most of these compounds appear not to have been previously reported in agricultural runoff. These compounds were present at concentrations below the few published aquatic toxicology data available; however, their potential to elicit more subtle effects in aquatic organisms cannot be excluded. None of these compounds were detected by broad-spectrum analysis in samples from the same fields during runoff-producing rain events.  相似文献   

18.
Flooded post-harvest rice paddies were examined as systems for reducing diazinon (organophosphate insecticide) concentrations in stormwater runoff. Two paddies were cultivated in Oryza sativa L. and amended with a 3-h simulated stormwater diazinon runoff event. Initial diazinon adsorption peaked at 347 and 571 μg kg?1 (3% mass load reduction) for mean above-ground plant tissue concentrations in each pond, respectively. Subsequent senescence of above-ground tissue showed significant decreases in tissue mass (r 2?=?0.985) and adsorbed diazinon mass (90?±?4% and 82?±?1%) within 1 month of amendment. There were no corollary increases in water column diazinon concentrations. Furthermore, control O. sativa tissue placed within the treatment ponds had below-detectable levels of diazinon throughout the decomposition phase, suggesting a lack of within pond transference of dissipated diazinon. This study shows the relative effectiveness of diazinon adsorption by post-harvest rice plants and a potential mitigation strategy of senescence and pesticide degradation for contaminated tailwater.  相似文献   

19.
The fate and transport of tricyclazole and imidacloprid in paddy plots after nursery-box application was monitored. Water and surface soil samples were collected over a period of 35 days. Rates of dissipation from paddy waters and soils were also measured. Dissipation of the two pesticides from paddy water can be described by first-order kinetics. In the soil, only the dissipation of imidacloprid fitted to the simple first-order kinetics, whereas tricyclazole concentrations fluctuated until the end of the monitoring period. Mean half-life (DT50) values for tricyclazole were 11.8 and 305 days, respectively, in paddy water and surface soil. The corresponding values of imidacloprid were 2.0 and 12.5 days, respectively, in water and in surface soil. Less than 0.9% of tricyclazole and 0.1% of imidacloprid were lost through runoff during the monitoring period even under 6.3 cm of rainfall. The pesticide formulation seemed to affect the environmental fate of these pesticides when these results were compared to those of other studies.  相似文献   

20.
Abstract

The diacetyl monoxime colorimetric method of determining urea in soil extracts was modified for microplate format. A 100‐μL aliquot of extract was treated with color reagent in a disposable plastic microtiter plate (96 wells/plate), and color was developed by heating the plate in a low‐temperature oven at 87°C for 55 min. After cooling for 20 min at ambient temperature, absorbance measurements were simultaneously performed on all 96 wells using a microplate reader. The microscale method was faster and more convenient than the conventional method; moreover, the volume of waste was markedly reduced. Studies to compare the two methods showed very little difference in accuracy, precision, or sensitivity.  相似文献   

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