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The development of instrumental analytics such as the LC-MS/MS has made it possible to quickly determine many component concentrations in a single chromatogram. However, the validation of such multi-methods needs new strategies for robustness and optimization. Statistical execution of analytical tests is one tool that can be utilized to meet this requirement. A Central Composite Design (CCD) was utilized for the validation of an LC-MS/MS multi-method for 84 analytes. The experimental design includes six design variables and two non-design variables (response variables). Concentration, ionization temperature, dwell time, gradient, flow (of eluent), and spraying/curtain gas (continuous design variables) were varied on five different levels; the whole design encompassed 91 runs. To investigate the robustness of a LC-MS/MS method both peak sensitivity and chromatographic separation had to be verified. Therefore, two non-design variables were necessary. The distribution of the peaks over analysis time was applied to describe the quality of the chromatographic separation. The sensitivity was described with the signal to noise ratio (S/N). The evaluation of the measured data was accomplished with the Analysis of Variance (ANOVA) and the Response Surface Methodology (RSM). Three main effects (concentration, ionization temperature, dwell time) and no significant interaction effect were found for the response variable “S/N”. The variables of concentration, ionization temperature, and dwell time had no significant effects for the response variable “S/N”. The ANOVA of the response variable chromatographic separation abandoned no significant effects as well. Therefore, robustness of the method can be guaranteed for all non significant design variables.  相似文献   
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The water quality of the Pozuelos-Murillo lagoon system in southern Mexico was evaluated during three periods between March and October 2002, with particular emphasis on the detection of organochlorine and organophosphorous pesticide residues in water and sediments. Physicochemical and microbiological parameters of water were also measured and integrated in a water quality index (WQI). Multivariate analysis was used to regionalise the lagoon system as a function of the behaviour of all measured parameters. Solid phase micro-extraction followed by gas chromatography (SPME-GC) was used for pesticide analysis. The concentration of phosphorous was found to be higher than that of nitrogenous compounds. This, besides a deficiency in dissolved oxygen and a high organic matter concentration (as COD), reflects eutrophication processes in some areas of the system. Measured levels of faecal coliforms and oils and greases were above the limits established by Mexican law and comparable to the concentrations reported for other highly polluted systems in Mexico. Residues of DDD (2.0 microg L(-1)) in water and DDE (247 ng g(-1)) and endosulfan I (814 ng g(-1)) sediments were detected by SPME-GC. The spatial distribution of these contaminants implies major potential risks because the most polluted sites were found to be those with the highest fishing activity. Although in general the WQI is on acceptable levels (65-80%), some contamination problems are evident.  相似文献   
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A collaborative sampling cruise off the central California coast was conducted to evaluate contaminant transport pathways along and across the shelf in the spring of 2002. The area has a complex current structure and net transport routes are not known for sure. Sediment characteristics, and organic and trace metal contaminants were analyzed in sediments taken from locations near shore, out to the heads of several canyons. Relative to the continental shelf and Pioneer Canyon stations, DDT was found at higher concentrations in Ascension and Monterey Canyons. Monterey Bay still receives DDT from terrestrial runoff and may be the source of DDT found in Ascension Canyon. DDT concentrations in Monterey Bay biota indicate bioaccumulation is occurring at depth due to continuing input from the shore. Effects on the deep ocean benthic community is unknown.  相似文献   
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Sediment and biota samples were collected from Msimbazi and Kizinga rivers and from the coastal marine environment of Dar es Salaam during both dry and wet seasons. The samples were analyzed for various organochlorine pesticide residues using GC-ECD and GC-MS. Dieldrin, p,p-DDT, p,p-DDE, p,p-DDD, o,p-DDT and γ-HCH were detected at significantly greater concentrations above the method detection limits. Recoveries of pesticide residues ranged 86.5–120% in sediments and 62–102% in biota. The average concentrations of total DDT in sediments for the two seasons were almost the same. Biota samples showed significant difference in levels of residues depending on mode of feeding and age of analyzed biota. p,p-DDT to total DDT ratios in all matrices indicated recent use of DDT. The levels of residues in sediments suggest possible adverse effects to humans consuming biota that are directly exposed to the sediments. This effect, which is associated with bio-concentration of residues in the tissues of edible aquatic biota, should not affect wildlife. In spite of concern on the adverse effect to humans posed by pesticide residues in sediments, edible biota from the examined water bodies were found to be safe for human consumption.  相似文献   
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The use of sequential measurements of hemolymph cholinesterase activities as a non-invasive biomarker of seasonal organophosphate/carbamate exposure was investigated for the tropical scallop, Euvola (Pecten) ziczac. Overall activities of both acetylcholinesterase and butyrylcholinesterase were relatively high compared to studies with bivalve tissues. Acute in vivo experiments showed inhibition of hemolymph acetylcholinesterase activity at concentrations of the organophosphate insecticide chlorpyrifos of 0.1, 1 and 10 ng l(-1). Monthly sampling of hemolymph from scallops at two sites in Bermuda over a 15 month period showed seasonal acetylcholinesterase and butyrylcholinesterase inhibition. Direct and indirect evidence suggests that this inhibition did not relate to biochemical or physiological changes associated with gonad maturation and spawning, but rather reflected diffuse contamination of the marine environment by cholinesterase inhibitors or increased bioavailability of such inhibitors at these times. Repetitive sampling of scallop hemolymph for cholinesterase activities represents a rapid, sensitive and non-invasive method for assessing seasonal, sublethal pesticide exposure in these commercially important bivalves and suggests a wider use in marine pollution monitoring.  相似文献   
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Contamination of groundwater has become a major concern in recent years. Since testing of water quality of all domestic and irrigation wells within large watersheds is not economically feasible, one frequently used monitoring strategy is to develop contamination potential maps of groundwater, and then prioritize those wells located in the potentially highly contaminated areas for testing of contaminants. However, generation of contamination potential maps based on groundwater sensitivity and vulnerability is not an easy task due inherent uncertainty. Therefore, the overall goal of this research is to improve the methodology for the generation of contamination potential maps by using detailed landuse/pesticide and soil structure information in conjunction with selected parameters from the DRASTIC model. The specific objectives of this study are (i) to incorporate GIS, GPS, remote sensing and the fuzzy rule-based model to generate groundwater sensitivity maps, and (ii) compare the results of our new methodologies with the modified DRASTIC Index (DI) and field water quality data. In this study, three different models were developed (viz. DIfuzz, VIfuzz and VIfuzz_ped) and were compared to the DI. Once the preliminary fuzzy logic-based (DIfuzz) was generated using selected parameters from DI, the methodology was further refined through VIfuzz and VIfuzz_ped models that incorporated landuse/pesticide application and soil structure information, respectively. This study was conducted in Woodruff County of the Mississippi Delta region of Arkansas. Water quality data for 55 wells were used to evaluate the contamination potential maps. The sensitivity map generated by VIfuzz_ped with soil structure showed significantly better coincidence results when compared with the field data.  相似文献   
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This paper develops mass fraction models for transport and fate of agricultural pollutants in structured two-region soils. Mass fraction index models, based on a semi-infinite domain solution, are derived that describe leaching at depth, vapor losses through soil surface, absorption, and degradation in the dynamic- and stagnant-water soil regions. The models predict that leaching is the result of the combined effect of the upward vapor-phase transport relative to downward advection, residence time relative to half-life, dispersion, and lateral diffusive mass transfer. Simulations show that leached fraction of volatile compounds does not always decrease monotonically with increased residence time relative to the pollutant half-life, as a result of complex interactions among the different physical and biochemical processes. The results show that leaching, volatilization, and degradation losses can be affected significantly by lateral diffusive mass transfer into immobile-water regions and advection relative to dispersion (i.e. Peclet number) in the mobile-water regions. It is shown that solute diffusion into the immobile phase and subsequent biochemical decay reduces leaching and vapor losses through soil surface. Potential use of the modified leaching index for the screening of selected pesticides is illustrated for different soil textures and infiltration rates. The analysis may be useful to the management of pesticides and the design of landfills.  相似文献   
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High resolution gas chromatography (HRGC) with ECD, NFID and MSD is a very efficient determination method for pesticides in water. Because of their relatively low concentrations in aquatic systems enrichment and preconcentration procedures are essential. Some examples for pesticide determination by GC methods are given. Potentials and limitations of HRGC for pesticide analysis are also discussed. An extensive pesticide analysis in water has to include different methods like HRGC, HPLC and GC/MS.  相似文献   
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