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1.
A continuation of an earlier interlaboratory comparison was conducted (1) to assess solid-phase extraction (SPE) using Empore disks to extract atrazine, bromacil, metolachlor, and chlorpyrifos from various water sources accompanied by different sample shipping and quantitative techniques and (2) to compare quantitative results of individual laboratories with results of one common laboratory. Three replicates of a composite surface water (SW) sample were fortified with the analytes along with three replicates of deionized water (DW). A nonfortified DW sample and a nonfortified SW sample were also extracted. All samples were extracted using Empore C(18) disks. After extraction, part of the samples were eluted and analyzed in-house. Duplicate samples were evaporated in a 2-mL vial, shipped dry to a central laboratory (SDC), redissolved, and analyzed. Overall, samples analyzed in-house had higher recoveries than SDC samples. Laboratory x analysis type and laboratory x water source interactions were significant for all four compounds. Seven laboratories participated in this interlaboratory comparison program. No differences in atrazine recoveries were observed from in-house samples analyzed by laboratories A, B, D, and G compared with the recovery of SDC samples. In-house atrazine recoveries from laboratories C and F were higher when compared with recovery from SDC samples. However, laboratory E had lower recoveries from in-house samples compared with SDC samples. For each laboratory, lower recoveries were observed for chlorpyrifos from the SDC samples compared with samples analyzed in-house. Bromacil recovery was <65% at two of the seven laboratories in the study. Bromacil recoveries for the remaining laboratories were >75%. Three laboratories showed no differences in metolachlor recovery; two laboratories had higher recoveries for samples analyzed in-house, and two other laboratories showed higher metolachlor recovery for SDC samples. Laboratory G had a higher recovery in SW for all four compounds compared with DW. Other laboratories that had significant differences in pesticide recovery between the two water sources showed higher recovery in DW than in the SW regardless of the compound. In comparison to earlier work, recovery of these compounds using SPE disks as a temporary storage matrix may be more effective than shipping dried samples in a vial. Problems with analytes such as chlorpyrifos are unavoidable, and it should not be assumed that an extraction procedure using SPE disks will be adequate for all compounds and transferrable across all chromatographic conditions.  相似文献   

2.
A multiresidue procedure was developed for analysis of cotton pesticide and harvest-aid chemicals in water using solid-phase extraction and analysis by GC-NPD, GC-MS, and HPLC-DAD. Target compounds included the defoliants tribufos, dimethipin, thidiazuron; the herbicide diuron; and the insecticide methyl parathion. Three solid-phase extraction (SPE) media, octadecylsilyl (ODS), graphitized carbon black (GCB), and a divinylbenzene-N-vinyl pyrollidine copolymer (DVBVP), were evaluated. On GCB and ODS, recoveries varied depending on compound type. Recoveries were quantitative for all compounds on DVBVP, ranging from 87 to 115% in spiked deionized water and surface runoff. The method detection limit was less than 0.1 microg L(-)(1). SPE with DVBVP was applied to post-defoliation samples of surface runoff and tile drainage from a cotton research plot and surface runoff from a commercial field. The research plot was defoliated with a tank mixture of dimethipin and thidiazuron, and the commercial field, with tribufos. Dimethipin was detected (1.9-9.6 microg L(-)(1)) in all research plot samples. In the commercial field samples, tribufos concentration ranged from 0.1 to 135 microg L(-)(1). An exponentially decreasing concentration trend was observed with each successive storm event.  相似文献   

3.
High-performance liquid chromatography (HPLC) methods for the determination of phenyl urea herbicides in water are described. The target compounds include chlortoluron, diuron, fluometuron, isoproturon, linuron, metobromuron, metoxuron, monuron, neburon, and siduron. Water was subjected to solid phase extraction (SPE) using either automated SPE with 47 mm C(18) Empore disks or on-line precolumn concentration. Herbicides were separated on a C(18) reversed phase column with an acetonitile-water gradient and were detected with either a diode array detector (DAD) or a postcolumn photolysis and derivatization (PPD) detector system. Photolysis converted the phenyl ureas to monoalkylamines that were derivatized to fluorescent isoindoles by reaction with o-phthalaldehyde and 2-mercaptoethanol. The DAD monitoring at 245 nm was linear over three decades with instrument detection limits of approximately 0.01 mg/L. SPE efficiency was between 48 and 70% in laboratory reagent water, but use of the internal standard quantitation method improved accuracy. High total dissolved solids and total organic carbon values in surface water improved recoveries relative to laboratory reagent water for all of the phenyl ureas. In Colorado River water spiked at 1 or 50 microg/L, mean recoveries ranged from 74 to 104%. Method detection limits (MDLs) ranged from 4 to 40 ng/L (parts per trillion) with the DAD instrument. PPD detection was highly specific but resulted in a slight loss in chromatographic efficiency and average MDLs approximately 5 times higher using a single set of detection conditions. The study indicates that methods based on SPE followed by HPLC with diode array or PPD detection have practical utility for trace analysis of phenyl ureas in drinking water or surface waters.  相似文献   

4.
Bar-Ilan  I.  Shmerkin  S.  Mingelgrin  U.  Levanon  D. 《Water, air, and soil pollution》2000,119(1-4):139-156
A survey was conducted of pesticide distribution in the water ofthe upper Jordan basin, due to the importance of its quality asthe main source of drinking water in Israel.A preliminary survey of pesticide distributers and farmersrevealed intensive use of many pesticides in agriculture. Fourof these were selected as targets for monitoring in the surfacewater of the region, at seven sampling stations. The highestresidue found was of aldicarb and its metabolites, with lowercontent of organophosphate and organochlorine insecticides. Noconcentrations reached the maximum levels permitted by the EPAfor drinking water, but recommendations were made, nonetheless,for continuous monitoring of pesticides in the region.Subsequent monitoring (1993–1997) showed a steady decrease in aldicarb residues.  相似文献   

5.
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   

6.
Solid-phase extraction (SPE) and direct competitive chemiluminescence enzyme immunoassay (dcCL-EIA) were combined for the detection of organophosphorus pesticides (OPs) in environmental water samples. dcCL-EIA based on horseradish peroxidase labeled with a broad-specificity monoclonal antibody against OPs was developed, and the effects of several physicochemical parameters on dcCL-EIA performance were studied. SPE was used for the pretreatment of water samples to remove interfering substances and to concentrate the OP analytes. The coupling of SPE and dcCL-EIA can detect seven OPs (parathion, coumaphos, phoxim, quinalphos, triazophos, dichlofenthion, and azinphos-ethyl) with the limit of quantitation below 0.1 ng/mL. The recoveries of OPs from spiked water samples ranged from 62.5% to 131.7% by SPE-dcCL-EIA and 69.5% to 112.3% by SPE-HPLC-MS/MS. The screening of OP residues in real-world environmental water samples by the developed SPE-dcCL-EIA and their confirmatory analysis using SPE-HPLC-MS/MS demonstrated that the assay is ideally suited as a monitoring method for OP residues prior to chromatographic analysis.  相似文献   

7.
Simple, rapid, and inexpensive methods have been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in drinking waters without interferences from other chemical contaminants by use of two different extraction techniques and analysis by an optimized reverse-phase (RP) high-performance liquid chromatography followed by fluorescence detection (HPLC-FLD) method. The feasibility of SPE (solid-phase extraction) and SPME (solid-phase microextraction) for the determination of PAH in drinking water samples has been evaluated. Several parameters have been studied and optimized for both extraction procedures. The relationship between the nature of the fibers and the quantity of extracted compounds and the effects of organic solvent, salt addition, sampling temperature, and sampling time was studied for SPME. Acetonitrile percentage added to the sample, sample storage conditions (temperature and time), and type of organic elution solvent and elution volume were evaluated for SPE. The results show that both extraction procedures can be used to determine PAHs in drinking waters, but SPE gives better performance (recovery, precision, and quantification limits) for the determination of PAHs in drinking water at the levels established by the legislation.  相似文献   

8.
Samples of raw and treated water were collected once in each of 3 seasons at 40 potable water treatment plants across Canada and were analyzed for phenol and 33 halogenated phenolic compounds including chlorophenols, bromophenols, bromochlorophenols, and chloroguaiacols. Eighteen of the compounds were not found at any treatment plant; phenol and each of the remaining halogenated phenols were found in at least 1 sample. Pentachlorophenol was the only halogenated phenolic compound found in more than 20% of the raw water samples in the fall and winter samples at levels up to 53 ng/L with mean values of 1.9 and 2.8 ng/L, respectively. No halogenated phenols were detected in raw water summer samples. The halogenated phenols found most frequently in treated water samples were 4-chloro-, 2,4-dichloro-, 2,4,6-trichloro-, and bromodichlorophenols. Mean values were less than 15 ng/L and maximum values seldom exceeded 100 ng/L. Most of the positive values for the treated water samples were found at 8 of the 40 treatment plants but no correlations could be found between halogenated phenol levels and raw water type, treatment process, or chemical dosages.  相似文献   

9.
遥感监测具有监测区域广、速度快、省时省力等优势,常用于大面积水质监测。其中,叶绿素a浓度是水质监测的一个重要指标。叶绿素a遥感反演的关键是建立遥感数据和叶绿素a含量的定量关系。本文选取石家庄市饮用水源地黄壁庄水库为研究区域,通过进行水体反射光谱现场测量和同步水质采样,得出研究区水体反射光谱特征,并采用丙酮分光光度法测得各水样中叶绿素a含量。在此基础上通过波段比值模型及一阶微分模型分别分析叶绿素a浓度与反射率之间的线性相关性。结果表明,黄壁庄水库各采样点水体叶绿素a浓度均在4.55μg·L-1以下,光谱反射率比值R705nm/R680nm和696 nm反射率的一阶微分值均与叶绿素a浓度有较显著的线性相关性(r2分别为0.736 6和0.875 5)。本文所得结论与方法可为未来对北方水库型水源地水体进行大面积遥感监测叶绿素a含量提供理论参考。  相似文献   

10.
In the present study, during a period of 16 months Colilert 3000 was validated in laboratory and field tests and compared to standard laboratory methods for monitoring of coliforms and E. coli. No false positive/negative results for coliforms/E. coli were found in 80 potable well water samples monitored with the Colilert 3000 and compared to standard methods. Although usage of Colilert 3000 to monitor raw water is not recommended by the manufacturer, the E. coli results of 100 samples were 100% positive by membrane filtration, Colilert 18 and MPN and only 80% positive by the Colilert 3000. In addition, in all positive samples, Colilert 3000 and Colilert 18 showed higher results of two to three orders of magnitude compared to MF and MPN. This significant difference was probably due to the presence of Aeromonas spp. and Vibrio spp. (natural inhabitants of the raw surface water) known to interfere with the Colilert test. Treated surface water was monitored by Colilert 3000 for the presence of coliforms and E. coli. Among the 100 samples tested in parallel by membrane filtration all were negative, while with Colilert 3000 only 76% were negative. Post-test identification of the positive samples did not reveal the presence of E. coli but interfering microorganisms. The last application was to evaluate Colilert 3000 to monitor accidental or deliberate pollution of drinking water with sewage sources. Among 20 samples spiked with raw sewage (0.1 and 1%) all results were positive for both coliforms and E. coli. The time span required for Colilert 3000 to detect positive samples was 6–10 h compared to 24 h with the standard membrane filtration.  相似文献   

11.
In this study, the concentrations of 15 perfluorinated compounds (PFCs) were analyzed in 30 water samples collected in Catalonia (Spain) at three stages of the drinking water treatment process in several water purification plants. In addition, the concentrations of 13 PFCs were determined in samples of fish and shellfish collected from coastal areas of Catalonia. The intake of PFCs through both pathways, drinking water intake and fish and shellfish consumption, was also estimated. In water samples, the highest mean concentrations corresponded to perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA) (1.81 and 2.40 ng/L, respectively), whereas perfluorodecanosulfonate (PFDS) and perfluorotetradecanoic acid (PFTDA) were under their respective limits of detection in all analyzed samples. The results show that although the current treatment processes caused slight reductions in PFC concentrations, these processes did not mean significant changes in the amounts of PFCs already contained in the raw water. Among the analyzed PFCs in fish and shellfish, only seven compounds could be detected in at least one composite sample. PFOS showed the highest mean concentration (2.70 ng/g fw), being detected in all species with the exception of mussels. With regard to PFOA (mean, 0.074 ng/g fw), the highest concentrations were detected in prawn and hake (0.098 and 0.091 ng/g fw, respectively). The current exposure to PFCs through consumption of fish and shellfish indicates that it should not be of concern for the consumers. The amounts ingested are well below the recommended tolerable daily intakes, at least for those PFCs for which information is available.  相似文献   

12.
The concentrations of 9 chlorinated pesticides in the water sources and tap waters of Istanbul, Turkey, were determined by gas chromatographic methods following the enrichment through adsorption and elution techniques. The observed organochlorine pesticides were α- and γ-HCH and aldrin which had been banned from use. The contents of α- and γ-HCH in raw waters were in the range of 0.34–1.7 ppb and not detected-0.077 ppb, respectively. Aldrin was observed at the concentration of 0.03 ppb in some samples. The residue levels of organochlorine pesticides in drinking water supplies of Istanbul were found significantly under the maximum permissible levels of standards. The effectiveness of potable water treatment processes and the importance of maintenance and back- washing of sand filters in pesticide removal were observed. Improper and delayed back-washings of filters caused an increase in the pesticide residues in the distributed water. In older water distribution lines, higher concentrations of some organochlorines were also observed.  相似文献   

13.
An interlaboratory method validation study was conducted on EPA Method 531.1, Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post Column Derivatization, to determine the precision and mean recovery for determination of 10 carbamate pesticide compounds in reagent water and in finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with 10 carbamate pesticides at 6 concentration levels, as 3 Youden pairs. Eight laboratories analyzed the samples by direct aqueous injection, with separation by reverse-phase liquid chromatography and post-column hydrolysis of the carbamates and carbamoyloximes to methylamine, followed by reaction of the methylamine with o-phthalaldehyde and 2-mercaptoethanol using fluorescence detection. Results were analyzed using an EPA computer program, which measured precision and recovery for each of the 10 compounds and compared the performance of the method between water types. The method was acceptable for all analytes tested. After removal of a nonrepresentative data set for aldicarb sulfoxide, no matrix effects were observed; the statistics for the pooled drinking waters were not significantly different from the statistics for the reagent waters. The method has been adopted official first action by AOAC.  相似文献   

14.
A new methodology is described for rapidly determining the herbicide oryzalin in water, citrus fruits, and stone fruits by liquid chromatography with negative ion electrospray ionization tandem mass spectrometry (LC/MS/MS). Oryzalin is extracted from water using a polymeric sorbent solid phase extraction (SPE) column and from fruit using methanol. The water samples require no further purification, but an aliquot of the fruit sample extracts is diluted with water and purified using a polymeric 96 well SPE plate. Purified extracts are concentrated prior to determination by LC/MS/MS at m/z 345 (Q1) and m/z 281 (Q3) using an external standard for calibration. The validated limits of quantitation were 0.05 microg/L in water (drinking water, surface water, and groundwater) and 0.01 microg/g in citrus fruits (oranges and lemons) and stone fruits (peaches and cherries). Recoveries averaged 102% for water samples and 85-89% for the various types of fruit samples. For all fortification levels combined, the relative standard deviations ranged from 4 to 6% for water and from 2 to 4% for fruit.  相似文献   

15.
Currently, regulatory practice in the United States is to estimate potential concentrations in drinking water from surface water by using an index reservoir scenario. This approach extrapolates results from the modeling of a single field with maximum application rates to the watershed scale, based on a percent crop area estimate. Since 1998, Bayer CropScience and its predecessor companies have conducted drinking water monitoring studies with a number of different compounds. The results from these studies show that the index reservoir scenario greatly overpredicts residues in surface water. The most important factor is the overestimation of use within a watershed. Other factors contributing to the overestimation of concentrations are the conservative procedures used to obtain the chemical fate related input parameters and the simplified hydrology. A new procedure based on the USGS WARP model, being developed by a group of scientists from the EPA, USGS, USDA, and industry, will provide more realistic estimates of concentrations of pesticides and their metabolites in drinking water.  相似文献   

16.
Crop-protection compounds are useful tools that enhance the quality of the food we enjoy. However, crop-protection products can enter aquatic systems either by direct or by indirect application. To better understand the possible frequency and magnitude of exposure to water resources, the regulatory community has developed a set of relatively straightforward models for estimating exposure to these water systems. The focus of this research was to compare how well the estimates of exposure to drinking water based on model calculations relate to actual monitoring data. Physical/chemical property data were entered in the EPA's exposure model FIRST and into PRZM/EXAMS. The predictions from FIRST and PRZM/EXAMS were then compared to actual monitoring data from a USGS/EPA cooperative program, which monitored for pesticides in vulnerable surface drinking water supplies during 1999 and 2000. Results from this examination indicate the exposure from the models can overpredict concentrations found in water by several orders of magnitude. An overprediction factor is presented that corrects model predictions to more closely approximate concentrations found in reservoirs (p = 0.05).  相似文献   

17.
Pesticide residues in foods are reported for the 4-year period 1982-1986 [fiscal years (FY) 83-86]. Results were summarized from the 2 complementary approaches that make up the Food and Drug Administration's (FDA) pesticide residue monitoring program. Under regulatory monitoring, which focuses on residues in raw agricultural commodities, a total of 49,055 samples (27,700 domestic and 21,355 import) that included fresh fruits and vegetables, grains and grain products, milk and dairy products, seafoods, and a variety of processed foods were analyzed. No residues were found in 60 and 48% of the domestic and import samples, respectively, compared with 55 and 44% in FY78-82. About 3% of the domestic and 5% of the import samples were violative. In FY78-82, about 3 and 7% were violative, respectively. The other FDA monitoring approach, the Total Diet Study, was revised in April 1982 to expand coverage of age/sex groups, use updated diets, and provide for analysis of individual foods. Results from monitoring under this modified approach and from regulatory monitoring continued to demonstrate that pesticide residues in the U.S. food supply were well below regulatory limits, and dietary intakes were many times lower than the Acceptable Daily Intakes established by international agencies.  相似文献   

18.
Because of the intensive use of pesticides for the control of certain pests in Egypt, country-wide residue monitoring programs must be established that can cover all the Egyptian Governorates exposed to pesticide treatments. To do so, limited programs must be adopted first, so that current situations and future needs for improved programs are identified. The present paper reports results from a limited monitoring program, which started in 1985 in one governorate and then expanded to include another in 1986. Fish and milk samples were the commodities selected for residue analysis. The results showed that milk samples collected from Beni-Suef Governorate in 1986 had lower levels of organochlorine residues compared to those collected in 1985. Residues in boltifish and catfish samples in 1986 were much higher than those detected in 1985. In comparison with Beni-Suef Governorate, and contrary to expectations, milk derived from Fayoum Governorate in 1986 was more contaminated with pesticides. While the amount of residues in boltifish was comparatively higher, catfish samples were less contaminated.  相似文献   

19.
Reduction of pesticide residues on produce by rinsing   总被引：6，自引：0，他引：6  
In 1997 this laboratory initiated a research program with the objective of examining the effect that rinsing of produce with tap water would have on pesticide residues. Samples were obtained from local markets and/or grown at our experimental farm. Because approximately 35% of produce from retail sources contains pesticide residues, growing and treating produce at an experimental farm had the advantage that all such samples contain pesticide residues. Pesticides were applied under normal field conditions to a variety of food crops and the vegetation was allowed to undergo natural weathering prior to harvest. The resulting samples contained field-incurred or "field-fortified" residues. This experimental design was employed to mimic as closely as possible real world samples. Crops were treated, harvested, and divided into equal subsamples. One subsample was processed unwashed, whereas the other was rinsed under tap water. The extraction and analysis method used was a multi-residue method developed in our laboratory. Twelve pesticides were included in this study: the fungicides captan, chlorothalonil, iprodione, and vinclozolin; and the insecticides endosulfan, permethrin, methoxychlor, malathion, diazinon, chlorpyrifos, bifenthrin, and DDE (a soil metabolite of DDT). Statistical analysis of the data using the Wilcoxon signed-rank test showed that rinsing removed residues for nine of the twelve pesticides studied. Residues of vinclozolin, bifenthrin, and chlorpyrifos were not reduced. The rinsability of a pesticide is not correlated with its water solubility.  相似文献   

20.
Formaldehyde is readily quantitated at micrograms/L levels in drinking water. The analyte present in 1 L water samples is derivatized with 2,4-dinitrophenylhydrazine in a 2M acid medium and then extracted with chloroform. After the solvent is exchanged for methanol, the product is separated and quantitated using reverse-phase liquid chromatography with UV detection (365 nm). Reporting limits as low as 20 micrograms/L (corrected for laboratory blank) are routinely achieved. Formaldehyde recovery typically exceeds 90% at 20-200 micrograms/L. The method was applied to hot and cold water samples from thirty-four 1- and 2-story houses equipped with poly(acetal) plumbing elbows and tees. The drinking water samples were accompanied by sets of blanks and spikes specified by a quality assurance/quality control plan. Formaldehyde was observed above the reporting limit in 80% of hot and cold water samples from the 1-story dwellings, but in less than 50% of those from the 2-story dwellings. The results may depend on both the construction of the houses (1- vs 2-story) and the time of year the water is sampled (mid-summer).  相似文献   

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