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1.
A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL−1 Ag+ in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL−1 for both Zn2+ and Cu2+, 80 μg·mL−1 for Pb2+, 1000 μg·mL−1 for Mn2+, and 100 μg·mL−1 for both Cd2+ and Ni2+. The calibration curve was linear in the range of 1–500 ng·mL−1 with a limit of detection (LOD) at 0.3 ng·mL−1. The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.  相似文献   

2.
Cloud point extraction (CPE) was used to simultaneously preconcentrate trace-level cadmium, nickel and zinc for determination by flame atomic absorption spectrometry (FAAS). 1-(2-Pyridilazo)-2-naphthol (PAN) was used as a complexing agent, and the metal complexes were extracted from the aqueous phase by the surfactant Triton X-114 ((1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol). Under optimized complexation and extraction conditions, the limits of detection were 0.37 μg L−1 (Cd), 2.6 μg L−1 (Ni) and 2.3 μg L−1 (Zn). This extraction was quantitative with a preconcentration factor of 30 and enrichment factor estimated to be 42, 40 and 43, respectively. The method was applied to different complex samples, and the accuracy was evaluated by analyzing a water standard reference material (NIST SRM 1643e), yielding results in agreement with the certified values.  相似文献   

3.
A method was developed for the quantification of araCTP, CTP and dCTP in a human follicular lymphoma cell line. This method involves solid phase extraction (SPE) using a weak anion-exchanger (WAX) cartridge, a porous graphitic carbon high-performance liquid chromatography (HPLC) column separation, and tandem mass spectrometry (MS/MS) detection. By using a triple quadrupole mass spectrometer operating in negative ion multiple reaction monitoring (MRM) mode, the method was able to achieve a lower limit of quantification (LLOQ) of 0.1 μg mL?1 for araCTP and of 0.01 μg mL?1 for both CTP and dCTP. The method was validated and used to determine the amount of araCTP, CTP and dCTP formed after incubation of araC and an araCMP prodrug in the human follicular lymphoma cell line RL.  相似文献   

4.
A simple and rapid method for the determination of seven phenothiazines derivatives (chlorpromazine, promethazine, levomepromazine, prochlorperazine, trifluoperazine, fluphenazine and thioridazine) in human urine samples is presented. The analytes are extracted from the sample in 50 μL of the ionic liquid 1-butyl-3-methyl-imidazolium hexafluorophosphate working in an automatic flow system under dynamic conditions. The chemical affinity between the extractant and the analytes allows a good isolation of the drugs from the sample matrix achieving at the same time their preconcentration. The separation and detection of the extracted compounds is accomplished by liquid chromatography and UV detection. The proposed method is a valuable alternative for the analysis of these drugs in urine within the concentration range 0.07–10 μg mL?1. Limits of detection were in the range from 21 ng mL?1 (thioridazine) to 60 ng mL?1 (levomepromazine). The repeatability of the proposed method expressed as RSD (n = 5) varied between 2.2% (levomepromazine) and 3.9% (chlorpromazine).  相似文献   

5.
New pre-concentration technique, triple phase suspended droplet microextraction (SD-LPME) and liquid chromatography-photodiode array detection was applied to determine ecstasy, MDMA (3,4-methylendioxy-N-methylamphetamine) in hair samples. In this research MDMA in hair was digested and after treatment extracted. The effective parameters were investigated and method was evaluated. Under the optimal conditions, the MDMA was enriched by factor 98.11. Linearity (r = 0.9921), was obtained in the range of 10–15,000 ng mL?1 and detection limit was 0.1 ng mL?1.  相似文献   

6.
The present study describes the simultaneous determination of four drugs, two local anaesthetics (lidocaine and bupivacaine) and two opium alkaloids (noscapine and papaverine) by capillary zone electrophoresis (CZE) with solid-phase extraction (SPE) procedure using Oasis HLB cartridges. Their recoveries ranged from 81 to 107% at the target concentrations of 2.0, 5.0 and 8.0 μg mL?1 in spiked urine samples. Coefficients of variation of the recoveries ranged from 2.1 to 11.3% at these concentrations. The quantitation limits of the method were approximately 300 ng mL?1 for the different compounds studied. The assay is very specific for these compounds and requires a short sample preparation procedure prior to the electrophoretic analysis.  相似文献   

7.
This paper describes the development of a two-dimensional, spatially distributed model to simulate coupled hydrologic and phosphorus (P) biogeochemical processes in a 147-ha cell of a 1544-ha stormwater treatment wetland designed to help protect the greater Everglades, FL, USA. The model was used to assess the effects of a suite of feasible management alternatives on the long-term ability of the wetland to sustain total P (TP) removal. The spatial and temporal dynamics of TP retention were simulated under historical (1995–2000) conditions, and under assumptions of removal of short-circuiting channels and ditches, changes in external hydraulic and TP loading, and long-term (>20 years) impacts on soil and water column TP dynamics under current and reduced load conditions. Internal hydrology and transport processes were calibrated against measured tracer concentrations, and subsequently validated against outflow discharge and spatial chloride concentration data. Cycling of P was simulated as first-order uptake and release, with different uptake coefficients for open water/sparse submerged aquatic vegetation (SAV) areas (0.2 day?1) and dense SAV areas (0.4 day?1), and a much lower, uniform release coefficient (1.97 × 10?4 day?1). The calibration and validation of the P model showed good agreement with field measurements of water column TP concentrations measured at the wetland outlet (calibration RMSE = 10.5 μg L?1; validation RMSE = 15.6 μg L?1). Under simulated conditions of preferential channels eliminated, average annual TP treatment effectiveness increased by 25%. When inflow TP loads were assumed to be eliminated after 6 years of loading, the release of accumulated soil P sustained predicted annual average outlet concentrations above 6.7 μg L?1 for 18 years, decreasing at a rate of 0.16 μg L?1 yr?1. Sensitivity analyses indicate that the most critical model input factors include flow resistance parameters, initial soil TP content, and P cycling parameters compared to initial water level, initial TP concentration in water column, ET and transport parameters.  相似文献   

8.
We studied for two years the seasonal changes in plant available nitrate and ammonium nitrogen (N), nitrification, N-mineralization, microbial biomass carbon (MBC), nitrogen (MBN) and phosphorus (MBP) in two forest and three cropland sites, derived from a tropical forest ecosystem of India. Results indicated that seasonal values of nitrate N, ammonium N and phosphate P ranged from 7.33–12.99, 5.1–10.22 and 4.0–7.8 μg g?1 in forest and 4.13–9.26, 9.35–14.46 and 2.8–5.8 μg g?1 in cropland ecosystems, respectively, with maximum values in summer and minimum in rainy seasons. Nitrification and N-mineralization values varied from 6–28 and 4–26 μg g?1 mo?1 in forest and 3–14 μg g?1 mo?1 and 4–17 μg g?1 mo?1 in cropland, with maximum values in rainy season and minimum in summer season.MBC, MBN MBP ranged from 393–753, 34–80 and 16–36 μg g?1 in forests and 186–414, 21–41 and 11–22 μg g?1 in croplands, being maximum in summer and minimum in rainy seasons. There was gradual increase in the values of inorganic N, nitrification, N-mineralization and MBC, MBN and MBP along the age of cropland. Analysis of variance indicated significant difference in the concentration of inorganic N, nitrification and N-mineralization and MBC, MBN and MBP due to sites and seasons.Cultivation caused decline in the mean annual organic C, N and P by 42%, 29% and 13%. The values of nitrate N were decreased by 23–38%, while ammonium N was increased by 39–74%. Nitrification and N-mineralization values were reduced by 39–63% and 40–60%, respectively. Microbial C, N and P were reduced by 44–54%, 41–50% and 28–44%, respectively. Nonetheless, the contribution of soil microbial biomass reflected in total N was enhanced from 4.76% in forest to 5.03% in cropland ecosystem. Enhancement of plant available ammonium-N and microbial contribution in total N are an indicator of natural conserving mechanism to check the nitrogen loss from the nutrient poor agro-ecosystem.  相似文献   

9.
Root cultures of Silybum marianum (L.) Gaertn. (Asteraceae) were established from in vitro germinated sterile plantlets. The cultures grew in hormone-free Murashige and Skoog medium. The flavonolignan content in the cultured roots was determined by HPLC using 30% acetonitrile in acidified water (0.5% phosphoric acid). The major flavonolignans produced by the cultured roots were silychristin (74.2 μg g?1 fresh weight (FW)) and silydianin (8.1 μg g?1 FW). The flavonolignan precursor taxifolin was also detected in the cultured roots (40.8 μg g?1 FW). Addition of methyl jasmonate to 7-days-old root cultures for 48 h increased the content of the produced flavonolignans and taxifolin to approximately 300% of the control cultures. Methyl jasmonate also enhanced about sixfold the accumulation of a compound identified as 3,3′,5,5′,7-pentahydroxyflavanone.  相似文献   

10.
Fermentation kinetics of growth and β-carotene production by Rhodotorula glutinis DM28 in batch and continuous cultures using fermented radish brine, a waste generated from fermented vegetable industry, as a cultivation medium were investigated. The suitable brine concentration for β-carotene production by R. glutinis DM28 was 30 g l?1. Its growth and β-carotene production obtained by batch culture in shake flasks were 2.2 g l?1 and 87 μg l?1, respectively, while, in a bioreactor were 2.6 g l?1 and 186 μg l?1, respectively. Furthermore, its maximum growth rate and β-carotene productivity in continuous culture obtained at the dilution rate of 0.24 h?1 were 0.3 g l?1 h?1 and 19 μg l?1 h?1, respectively, which were significantly higher than those in the batch. Therefore, improved growth rate and β-carotene productivity of R. glutinis in fermented radish brine could be accomplished by continuous cultivation.  相似文献   

11.
Selenium (Se) is a metalloid that can occur naturally in soils from the Cretaceous shale deposits of a prehistoric inland sea in the western United States. Agricultural irrigation and runoff solubilizes Se from these shales, causing buildups of toxic levels of selenate (SeO42−) in water and soil. Our main objective was to investigate the accumulation of Se in two Brassicaceae species chosen for their potential as phytoremediators of Se contaminated soils. We tested the hypothesis that Se will accumulate in the pollen and nectar of two plant species and negatively affect floral traits and plant reproduction. Certain species of Brassicaceae can accumulate high concentrations of Se in their leaf tissues. In this study Se accumulation in plant tissues was investigated under greenhouse conditions. Se accumulator (Brassica juncea) and Se hyperaccumulator (Stanleya pinnata) plants were irrigated in sand culture with 0 μM selenate (control), 8 μM selenate, and 13 μM selenate.Nectar and pollen in S. pinnata contained up to 150 μg Se mL−1 wet weight and 12900 μg Se g−1 dry weight when irrigated with 8 μM selenate. Se levels in nectar (110 μg Se mL−1 wet weight) and pollen (1700 μg Se g−1 dry weight) were not as high in B. juncea. Floral display width, petal area and seed pod length were significantly reduced in the 13 μM selenate Se treatment in B. juncea. S. pinnata floral traits and seeds were unaffected by the Se treatments.This study provides crucial information about where some of the highest concentrations of Se are found in two phytoremediators, and may shed light on the potential risks pollinators may face when foraging upon these accumulating plants. In the field, duration of the plant's exposure, Se soil and water concentrations as well as other environmental factors may also play important roles in determining how much Se is accumulated into the leaf and floral tissues. Our greenhouse study shed light on two species’ ability to accumulate Se, as well as determined the specific plant tissues where Se concentrations are highest.  相似文献   

12.
The toxic effects of Aroclor 1254 (0.05, 0.5, 5 and 50 μg l?1) on scallop (Chlamys farreri) immune system in vivo were studied. The results showed that Aroclor 1254 had significant toxic effect on the parameters tested in this paper (P < 0.05). The total number of haemocytes, the proportion of granulocytes, phagocytosis in all groups as well as the lysosomal membrane stability (LMS) in 5, 50 μg l?1 and bacteriolytic activity 0.5, 5, 50 μg l?1 treatments decreased significantly, while the proportion of hyalinocytes and the production of O2- in all treatments remarkably increased during the sampling time and tended to be stable gradually after 6–15 d. The bacteriolytic activity in 0.05 μg l?1 treatments, LMS in 0.05, 0.5 μg l?1 groups and the DNA damage (comet ratios and arbitrary values) in all treatments increased at the beginning of exposure and reached their peaks on day 1, day 1, day 6 and day 3, following that they all decreased gradually and became stable after 9–15 d. When the indices reached stability, except for DNA damage was higher than controls, the others were all significantly lower than those of controls (P < 0.05). Thus, Aroclor 1254 has evident toxic effects on scallop immune system, which supports the view that a relationship exists between pollution and immunomodulation in aquatic organisms. Also it supports the speculation that the PCBs pollution is one of the important reasons of the mass mortality of the C. farreri.  相似文献   

13.
The effect of long-term (30 days) exposure to PCZ (0.2, 50, and 500 μg l?1) on intestine-related biochemical markers in rainbow trout was investigated. Multiple biomarkers were measured, including digestive enzymes (proteolytic enzymes and amylase), antioxidant responses (TBARS, CP, SOD, CAT, GR and GPx) and energy metabolic parameters (RNA/DNA ratio, Na+-K+-ATPase). Exposure to 500 μg l?1 PCZ led to significantly inhibited (p < 0.01) proteolytic enzyme and amylase activity. Activities of the antioxidant enzymes SOD, CAT, and GPx gradually increased at lower PCZ concentrations (0.2 and 50 μg l?1). At the highest concentration (500 μg l?1), oxidative stress was apparent as significant higher (p < 0.05) lipid peroxidation and protein carbonyls, associated with an inhibition of antioxidant enzymes activity. Moreover, energy metabolic parameters (RNA/DNA ratio, Na+-K+-ATPase) were significantly inhibited (p < 0.01) in the intestines of fish exposed to 500 μg l?1 PCZ, compared with controls. We suggest that long-term exposure to PCZ could result in several responses in intestine-related biochemical markers, which potentially could be used as indicators for monitoring residual PCZ present in the aquatic environment.  相似文献   

14.
Microbial nuclease P1 from Penicllium citrinum was immobilized on macroporous absorbent resins: strong polar poly (styrene-co-DVB) resin (SPPSD), polymethacrylic ester resin and poly (styrene-co-DVB)-Br resin. The results showed that SPPSD was the best carrier. Three methods of glutaraldehyde cross-linking were used and simultaneous immobilization and cross-linking (CIS) was demonstrated to be the best method. The functional properties of immobilized nuclease P1 were studied and compared to those of the free enzyme. The highest enzyme activities of free and immobilized nuclease P1 were obtained in 0.2 M acetate buffer at pH 4.5 and a temperature of 70 °C. An increase in Km (from 3.165 to 18.125 mg mL?1) and a decrease in Vmax (from 1667.18 to 443.95 U min?1 mL?1) were recorded after immobilization. SPPSD-glutaraldehyde-nuclease P1 exhibited better thermal stability than the free enzyme. The apparent activation energy (Ea) of the free and immobilized nuclease P1 was 137.04 kJ mol?1 and 98.43 kJ mol?1, respectively, implying that the catalytic efficiency of the immobilized enzyme was restricted by mass-transfer rather than kinetic limit.  相似文献   

15.
A rapid method has been developed to analyse CP 47, 497 in human urine. Urine samples were diluted with water:acetonitrile (90:10, v/v) and sample aliquots were analysed by triple quadrupole tandem mass spectrometry with a runtime of 5 min. Multiple reaction monitoring (MRM) as survey scan was performed. The method was validated in urine, according to an in-house validation protocol based on the criteria defined in Commission Decision 2002/657/EC. Three MRM transitions were monitored. The decision limit (CCα) was 0.01 μg mL?1 and for the detection capability a (CCβ) value of 0.02 μg mL?1 was obtained. The measurement uncertainty of the method was 21%. Fortifying human urine samples (n = 18) in three separate assays, show the accuracy of the method to be between 95 and 96%. The precision of the method, expressed as RSD values for the within-lab reproducibility at the three levels of fortification (0.1, 0.15 and 0.2 μg mL?1) was less than 10% respectively. The method proved to be simple, robust and time efficient. To the best of our knowledge there are no LC–MS methods for the determination of CP 47, 497 with validation data in urine.  相似文献   

16.
The study present evaluated the levels of mercury (Hg) and methylmercury (MeHg) in hair samples of people from Barreiras community, riverside inhabitants of the Tapajós River (Pará, Brazil), an area impacted by clandestine gold mining, as well as we analyzed the levels of Hg and Se (selenium) in nine fish species (carnivores and non-carnivorous) from the Tapajós River, which stand out as the main species consumed by riverside inhabitants, to evaluate a relationship between frequency of fish consumption and Hg concentration, and also to evaluate possible mechanisms of fish protection (or non-protection) to Hg exposure by Se. Furthermore we analyze the water quality to evaluate the environmental trophic state, fact responsible by creating conditions that can potentiate the effects of toxic mercury. Concentrations of Hg and MeHg were analyzed in hair samples of 141 volunteers in different age band. Of those, 84.40% of samples present values above the threshold for biological tolerance, which is 6.00 μg g−1 of total Hg in hair. Total Hg, in men there was a variation of 2.07–24.93 μg g−1, while for women the variation was 4.84–27.02 μg g−1. Consequently, the level of MeHg in men presented a variation of 1.49–19.57 μg g−1, with an average of 11.68 μg g−1, while with women the variation was from 3.73 to 22.35 μg g−1, with an average of 10.38 μg g−1. In fish species, Hg concentrations in carnivorous species had an average of 0.66 μg g−1, higher than that permitted by current legislation, ranging from 0.30 to 0.98 μg g−1, while the non-carnivorous species have values below the recommended by the legislation averaging 0.09 μg g−1, ranging between 0.02 and 0.44 μg g−1. For Se in fish, show that among carnivores, the contents of Se ranged between 0.18 and 0.54 μg g−1 with a mean of 0.34 μg g−1, while for non-carnivores these values were of the order of 0.16–0.56 μg g−1, with an average of 0.32 μg g−1. In surface water quality variables at the sampling points all showed values in accordance with the range established by current legislation. In this regard, the results provided by this study, while not conclusive, are strong indicators that despite not having been shown the relationship between the concentration of mercury in hair and feeding habits along the Tapajós River basin communities showed that a plausible correlation exists between levels of mercury and selenium in fish. This fact may serve as a subsidy to research human health, because in the Amazon, there is still a lot to examine with regards to the full understanding of the Se cycle.  相似文献   

17.
《Journal of Asia》2014,17(3):287-293
The efficacy of an essential oil obtained from Pimpinella anisum fruits and its major compound, trans-Anethole, was tested on the eggs, larvae and adults of Culex quinquefasciatus. While causing no significant mortality on eggs, other tested stages were very sensitive to the essential oil and trans-Anethole. LC50 for the 2nd to 4th instar larvae was estimated as 26–27 μL·L 1 and 15–19 μL·L 1 for the essential oil and trans-Anethole, respectively. As for the essential oil applied on adults, LC(LD)50 was estimated as 9.3 μL mL 1 (spray test), 1.9 μL L 1 (fumigation test) and 0.6 μg cm 2 (tarsal test), and for trans-Anethole as 8.1 μL mL 1 (spray test), 2.1 μL L 1 (fumigation test) and 0.4 μg cm 2 (tarsal test). The time needed to achieve 50% mortality after application of LC(LD)99 of the essential oil was significantly different; for example, in larvicidal assays it ranged from 15 to 235 min depending on the larval instar, and from 9 to 180 min when applied to adults, depending on the mode of application. It was also found that temperature had an important effect on the larvicidal efficacy of the essential oil, and oviposition deterrent activity was studied.The essential oil and trans-Anethole were toxic for Daphnia magna (62–92% mortality) and significantly reduced its fertility at high concentrations (35–50 μL mL 1) and long exposure (48 h). However, no negative effect on Daphnia mortality or fertility was found at shorter exposure times (6 h) and/or lower concentrations (20 μL mL 1).Based on the results of this study, we can recommend the essential oil from P. anisum as a suitable active substance for potential botanical insecticides.  相似文献   

18.
The concentration of lead in liver and kidneys of Wistar rats, fed with lead since fetal period in relation to their age and to a control group, was determined. A group of rats was exposed to lead acetate (n = 30) in drinking water and the other group was exposed to normal water (n = 20). Samples were collected from rats aging between 1 and 11 months and were analyzed by Energy Dispersive X-ray Fluorescence (EDXRF) without any chemical preparation. The EDXRF results were assessed by the PIXE (Proton Induced X-ray Emission) technique. The formaldehyde used to preserve the samples was also analyzed by ETAAS (Electro-Thermal Atomic Absorption Spectrometry) in order to verify if there was any loss of lead from the samples to the formaldehyde. We found that the loss was not significant (<2%).Concerning the mean values of the lead concentration measured in the contaminated soft tissues, in liver they range from 6 to 22 μg g?1, and in kidneys from 44 to 79 μg g?1. The control rats show, in general, values below the EDXRF detection limit (2 μg g?1). The ratio kidney/liver ranges from 2 to 10 and is strongly positively correlated with the age of the animals. A Spearman correlation matrix to investigate the correlation between elemental concentrations and the dependence of these concentrations with age showed that there is a strong positive correlation with age for lead in the liver but not in the kidney. The correlation matrix showed also that the concentration of lead in these two soft tissues is not correlated. The lead accumulation in liver is made by different plateaus that strongly decrease with age. It was verified the existence of two levels of accumulation in kidney, not very highlighted, which might be indicative of a maximum accumulation level for lead in kidney.  相似文献   

19.
Penicillium sp. F37 has been isolated from the marine sponge Axinella corrugata and shown to be closely related to Penicillium maximae. From the culture of Penicillium sp. F37 arvoredol, a novel chlorinated polyketide with 6,7-dihydro-4(5H)-benzofuranone moiety has been isolated and characterized by spectroscopic methods Arvoredol prevented biofilm formation of the human pathogen Staphylococcus epidermidis at a concentration of 125 μg mL−1 by 40%. It was also active against colorectal carcinoma HCT116 cells with a MIC of 7.9 μg mL−1.  相似文献   

20.
In this study, a membrane biofilm reactor performance for toluene as a model pollutant is presented. A composite membrane consisting of a porous polyacrylonitrile (PAN) support layer coated with a very thin (0.3 μm) dense polydimethylsiloxane (PDMS) top layer was used. Batch experiments were performed to select an appropriate inocula (slaughterhouse wastewater treatment sludge with a specific toluene consumption rate of 118 ± 23 μg g?1 VSS L?1) among the three available sources of inoculums. The maximum elimination capacity gas-side reactor volume based (EC)v and membrane based (EC)m, max obtained were 609 g m?3 h?1 and 1.2 g m?2 h?1 respectively, which is much higher than other membrane bioreactors. Further experiments involved the study of the membrane biofilm reactor flexibility when operational parameters as temperature, loading rate etc. were modified. In all cases, the membrane biofilm reactor showed a rapid adaptation and new steady-states were obtained within hours. Overall, the results illustrate that membrane bioreactors can potentially be a good option for treatment of air pollutants such as toluene.  相似文献   

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