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1.
An adsorptive differential pulse stripping method for the simultaneous determination of lead and tin is proposed. The procedure involves an adsorptive accumulation of lead and tin on a hanging mercury drop electrode (HMDE), followed by oxidation of adsorbed lead and tin by voltammetric scan using differential pulse modulation. The optimum experimental conditions are: 0.2 mol L?1 HNO3, accumulation potential of ?900 mV versus Ag/AgCl, accumulation time of 200 s, scan rate of 20 mV s?1 and pulse height of 80 mV. Lead and tin peak currents were observed in the same potential region at about ?400 mV. The simultaneous determination of lead and tin by using voltammetry is a difficult problem in analytical chemistry, due to voltammogram interferences. The resolution of a mixture of lead and tin by the application of orthogonal signal correction‐partial least squares (OSC‐PLS) was performed. The linear dynamic ranges were 0.003‐0.35 and 0.008‐0.50 μg mL?1 and detection limits were land 3 ng mL?1 for lead and tin, respectively. The RMSEP for lead and tin with OSC and without OSC were 2.8737, 6.0557 and 8.0941, 9.5151, respectively. The capability of the method for the analysis of real samples was evaluated by the determination of lead and tin in water samples with satisfactory results.  相似文献   

2.
To address drug resistance to influenza virus neuraminidase inhibitors (NAIs), a series of novel boron-containing N-substituted oseltamivir derivatives were designed and synthesized to target the 150-cavity of neuraminidase (NA). In NA inhibitory assays, it was found that most of the new compounds exhibited moderate inhibitory potency against the wild-type NAs. Among them, compound 2c bearing 4-(3-boronic acid benzyloxy)benzyl group displayed weaker or slightly improved activities against group-1 NAs (H1N1, H5N1, H5N8 and H5N1-H274Y) compared to that of oseltamivir carboxylate (OSC). Encouragingly, 2c showed 4.6 times greater activity than OSC toward H5N1-H274Y NA. Moreover, 2c exerted equivalent or more potent antiviral activities than OSC against H1N1, H5N1 and H5N8. Additionally, 2c demonstrated low cytotoxicity in vitro and no acute toxicity at the dose of 1000 mg/kg in mice. Molecular docking of 2c was employed to provide a possible explanation for the improved anti-H274Y NA activity, which may be due to the formation of key additional hydrogen bonds with surrounding amino acid residues, such as Arg152, Gln136 and Val149. Taken together, 2c appeared to be a promising lead compound for further optimization.  相似文献   

3.
Microcalorimetric isothermal monitoring was carried out for compost and compost-containing growing medium, to provide fingerprints of compost microbial activity at different conditions. Microbial activity is a key property of composts used in agricultural practice. Two aspects are addressed in this study: (1) microcalorimetric evaluation of compost response to glucose as a model stimulating agent; (2) examination of the impact of compost pre-drying and re-wetting on its biological activity.

Addition of glucose solution to the compost involved a strong increase in microbial activity, which was associated with a significant heat evolution without a lag period. In certain cases, this heat evolution was of complicated shape thus manifesting the heterogeneity of microbial populations in composts. Relation between cumulative energy evolved and the amount of added glucose was found to be helpful in distinguishing between aerobic and anaerobic regime of compost microbial activity. As distinct from non-dried compost or growing mixture, glucose addition to samples pre-dried at 65 °C resulted in delayed heat response with initial exponential-like heat evolution. This delay in heat evolution suggests that biological activity was significantly suppressed upon compost drying. Such a temperature-induced inactivation process might also result in dominance of a relatively homogeneous microbial population which survived the heating, thus involving a smooth, exponential-like initial step of the heat evolution. Noteworthy, addition of water (without glucose) to pre-dried compost results in an outburst of activity as compared with non-dried compost. This heat evolution outburst was also characterized by a lag period and an initial exponential-like phase. The heat evolution obtained with pre-dried compost upon water addition was not related to the compost wetting energy but rather reflected the formation of new carbon source due to the changes in compost organic matter upon heating or to the dead biomass of those microbial populations that did not resist the compost heating/drying.  相似文献   


4.
A liquid chromatography–tandem mass spectrometry method for the analysis of seven antiviral drugs, zanamivir, ribavirin, oseltamivir, oseltamivir carboxylate, amantadine, rimantadine and arbidol, in poultry muscle is reported. The antiviral drugs were extracted from the homogenized poultry muscle sample using methanol. The extract was purified using tandem solid-phase extraction combining a cation exchange cartridge and a phenylboronic acid cartridge. To prevent excessive matrix effects, the analytes were separated from the matrix constituents using a column-switch liquid chromatography system combining a reversed-phase and a Hypercarb analytical column. Detection was carried out using tandem mass spectrometry. The method was fully validated according to 2002/657/EC [1] and proved to be adequate for quantification and confirmation of zanamivir and ribavirin at 10 μg kg−1, oseltamivir, oseltamivir carboxylate, amantadine and rimantadine at levels below 1.0 μg kg−1 and for qualitative confirmatory analysis of arbidol at levels below 1 μg kg−1.  相似文献   

5.
The method of protein-based stable isotope probing (protein-SIP) has previously been shown to allow the modeling of carbon fluxes in microbial communities, thus tackling one of the key questions in microbial ecology. The method allows the analysis of stable isotope distribution in peptides, revealing metabolic activities of the species present in an ecosystem. Besides carbon, an application of protein-SIP with nitrogen is of interest for resolving the nitrogen fluxes in microbial communities. Thus, the sensitivity and reliability of a protein-SIP approach employing 15N was analyzed. For this, cultivations of Pseudomonas fluorescens ATCC 17483 with different ratios of 14N/15N were performed, from 10 % down to 0.1 % 15N. After incubation leading to complete labeling of biomass, proteins were extracted and separated by one-dimensional gel electrophoresis, followed by tryptic digest and UPLC Orbitrap MS/MS analysis. 15N relative isotope abundance (RIA) was calculated based on isotopic patterns from identified peptides in mass spectra. Proteomics data have been deposited to ProteomeXchange with identifier PXD000127. The distribution of 15N RIA values among peptides was analyzed in samples with different 15N amount, and potential causes for variations within individual samples of either technical or biological origin were investigated. Using a number of 50 peptides, significant differences (p?≤?0.05) in 15N incorporation were found between samples of different 15N RIA down to 0.1 %. The study demonstrates that protein-SIP using 15N is sufficiently sensitive for quantitative investigation of microbial activity in nitrogen cycling processes.  相似文献   

6.

Paraquat dichloride commonly used as herbicide was determined by differential pulse cathodic stripping voltammetry technique. Experimental parameters, such as pH, accumulation time, accumulation potential and initial potential were optimized. In this analysis, paraquat dichloride exhibited a well-defined tworeduction peaks at ?0.35 and ?0.90 V in the pH range from 2.0 to 12.0. The 0.04 mol L–1 BR buffer at pH 2.0 was found a suitable medium for electroanalytical determination of the paraquat dichloride. Interfering ions effect was not significant. Linear calibration plots for standard solutions of paraquat dichloride were obtained in the range of 0.25 to 1.75 × 10–6 mol L–1. Detection limit was 3.66 × 10–8 mol L–1. The optimized parameters were effectively applied for the determination of commercial paraquat dichloride and in artificial samples. Artificial samples were prepared by spiking paraquat dichloride into tap water and drinking water dispenser samples. The recovery value was 90.5% in drinking water dispenser samples and 91.7% in tap water samples at the concentration range of 1.00 × 10–6 to 1.75 × 10–6 mol L–1.

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7.
A mesoporous silica was synthesised and used to modify the surface of carbon paste electrode (CPE). The electrochemical behaviours of p-aminophenol were investigated. Compared to the unmodified CPE, the mesoporous silica-modified CPE obviously lowers the oxidation potential of p-aminophenol, and remarkably increases its oxidation peak current. The effects of pH value, amount of mesoporous silica, accumulation potential and time were examined. As a result, a sensitive, rapid and convenient electroanalytical method was developed for p-aminophenol. The linear range is from 0.025?mg?L?1 to 3?mg?L?1, and the limit of detection is 0.01?mg?L?1 after 2-min accumulation. Finally, the method was successfully used to determine p-aminophenol in water samples.  相似文献   

8.
Ribavirin is a synthetic, broad-spectrum antiviral drug. Ribavirin is recommended as an antiviral drug in the Interim Guidance for Diagnosis and Treatment (the seventh edition) of COVID-19. The ribavirin levels in red blood cells may be closely related to both its efficacy and adverse drug reactions. In this study, a simple and fast HPLC–UV method was established to determine the concentrations of total ribavirin in the red blood cells of 13 patients with COVID-19. Phosphorylated ribavirin was dephosphorylated by phosphatase incubation to obtain the total amount of ribavirin in red blood cells. The chromatographic column was an Atlantis C18. The recoveries were 85.45–89.05% at three levels. A good linear response was from 1 to 200 μg/ml, with a correlation coefficient of r2 = 0.9991. The concentration of total ribavirin in the red blood cells of the patients ranged from 30.83 to 133.34 μg/ml. The same samples without phosphatase incubation ranged from 4.07 to 20.84 μg/ml. About 85% of ribavirin was phosphorylated in red blood cells. In addition, we observed changes in these patients' hematological parameters and found that the erythrocyte, hemoglobin and hematocrit declined to the lowest levels on the fifth day after discontinuation of ribavirin (p < 0.05).  相似文献   

9.
The main objective of this work is the accurate measurement of uranium in the potable water sources of Muktsar district of Punjab, India. In the present work, a laser fluorimetry technique was used for the analysis of uranium. Inductively coupled plasma mass spectrometry (ICPMS) technique was also applied to verify and compare the uranium content analyzed using laser technique. About 16 samples from waterworks, bore wells, and hand pumps that supply the drinking water to local population were collected for this purpose. An indigenous laser fluorimeter supplied by RRCAT, Indore was employed for the analysis. Uranium concentrations obtained were in the range from 0 to 10???g?L?1 in ten samples, 11?C30???g?L?1 in three samples, and more than 100???g?L?1 in three samples namely Channu ground water, Warning Khera pump, and Killanwale village hand pump. The USEPA guideline value for uranium in safe drinking water is 30???g?L?1. Also, a data comparison with similar studies carried out in other countries is presented.  相似文献   

10.
Experiments on the removal and recovery of U(VI) from aqueous solution by tea waste were conducted. The adsorbent was characterized by scanning electron microscope and energy dispersive spectrometer before and after the adsorption treatment. The removal of U(VI) amounts to 86.80?% at optimum pH 6. The adsorption process reaches its equilibrium in 12?h at 308?K, and the kinetic characteristic can be described by the pseudo-second-order kinetic equation. The amount of adsorption increases from 22.92 to 142.21?mg?g?1 with the decrease of tea waste dosage from 100 to 10?mg for solution with an initial uranium concentration of 50?mg?L?1. Desorption for the four strippants is higher than 80?%. The equilibrium data are more agreeable with Freundlich isotherm than Langmuir isotherm.  相似文献   

11.
This work describes the development by response surface methodology (RSM) of a procedure for copper determination by inductively coupled plasma optical emission spectrometry (ICP OES) in water samples after extraction by copper imprinted polymer. Results of the two-level full factorial design (24) based on an analysis of variance demonstrated that only the solution pH; amount of polymer and adsorption time were statistically significant. Optimal conditions for the extraction of copper samples were obtained by using Box-Behnken design. Solution pH; amount of polymer and adsorption time were regarded as factors in the optimisation study. The working conditions were 4.6, 0.03?g and 3.5?h, for solution pH, amount of polymer; and adsorption time, respectively. Under the optimised experimental conditions, the detection limit of the proposed method followed by ICP OES was found to be 0.8?µg?L?1. The relative standard deviation (RSD) was found to less than 0.81%. The pre-concentration factor was 22.5. The accuracy of the optimised procedure was evaluated by analysis of certified reference material. The method was applied to the determination of copper in water samples.  相似文献   

12.
The design of narrow band gap (NBG) donors or acceptors and their application in organic solar cells (OSCs) are of great importance in the conversion of solar photons to electrons. Limited by the inevitable energy loss from the optical band gap of the photovoltaic material to the open‐circuit voltage of the OSC device, the improvement of the power conversion efficiency (PCE) of NBG‐based OSCs faces great challenges. A novel acceptor–donor–acceptor structured non‐fullerene acceptor is reported with an ultra‐narrow band gap of 1.24 eV, which was achieved by an enhanced intramolecular charge transfer (ICT) effect. In the OSC device, despite a low energy loss of 0.509 eV, an impressive short‐circuit current density of 25.3 mA cm−2 is still recorded, which is the highest value for all OSC devices. The high 10.9 % PCE of the NBG‐based OSC demonstrates that the design and application of ultra‐narrow materials have the potential to further improve the PCE of OSC devices.  相似文献   

13.
The design of narrow band gap (NBG) donors or acceptors and their application in organic solar cells (OSCs) are of great importance in the conversion of solar photons to electrons. Limited by the inevitable energy loss from the optical band gap of the photovoltaic material to the open‐circuit voltage of the OSC device, the improvement of the power conversion efficiency (PCE) of NBG‐based OSCs faces great challenges. A novel acceptor–donor–acceptor structured non‐fullerene acceptor is reported with an ultra‐narrow band gap of 1.24 eV, which was achieved by an enhanced intramolecular charge transfer (ICT) effect. In the OSC device, despite a low energy loss of 0.509 eV, an impressive short‐circuit current density of 25.3 mA cm−2 is still recorded, which is the highest value for all OSC devices. The high 10.9 % PCE of the NBG‐based OSC demonstrates that the design and application of ultra‐narrow materials have the potential to further improve the PCE of OSC devices.  相似文献   

14.
The yield of methyl methacrylate (MMA) polymerization as a function of triethylaluminum (TEA) concentration for a constant azobisisobutyronitrile (AIBN) concentration at 50°C has been measured. The polymerization yield does not differ markedly from that with AIBN alone as long as the initial TEA concentration is held smaller than four times the initial AIBN concentration. A sudden decrease in yield and molecular weight is observed at TEA/AIBN concentration ratios between 4 and 5. A plot of M?w?1 vs. TEA gives a rate-transfer constant of 89 1./mole-sec. If the reaction mixture is vacuum-evaporated with a previous addition of water, instead of precipitating the polymer, the formation of a considerable amount of MMA oligomer is detected for TEA/AIBN concentration ratios larger than 4. On the average, each TEA molecule in excess of four times the initial amount of AIBN yields one oligomer molecule. The data are consistent with a radical polymerization mechanism for the high molecular weight polymer and with a nonradical one for the oligomer formation.  相似文献   

15.
A cloud point extraction procedure for pre-concentration and determination of cadmium and lead in drinking water using sequential multi-element flame atomic absorption spectrometry is described. 4-(2-thiazolylazo)-orcinol (TAO) has been used as complexing agent and the micellar phase was obtained using the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) and centrifugation. The conditions for reaction and extraction (surfactant concentration, reagent concentration, effect of incubation time, etc) were studied and the analytical characteristics of the method were determined. The method allows the determination of cadmium and lead with quantification limits of 0.30?µg?L?1 and 2.6?µg?L?1, respectively. A precision expressed as relative standard deviation (RSD, n?=?10) of 2.3% and 2.6% has been obtained for cadmium concentrations of 10?µg?L?1 and 30?µg?L?1, respectively, and RSD of 1.3% and 1.7% for lead concentrations of 10?µg?L?1 and 30?µg?L?1, respectively. The accuracy was confirmed by analysis of a natural water certified reference material. The method has been applied for the determination of cadmium and lead in drinking water samples collected in the cities of Ilhéus and Itabuna, Brazil. Recovery tests have also been performed for some samples, and results varied from 96 to 105% for cadmium and 97 to 106% for lead. The cadmium and lead concentrations found in these samples were always lower than the permissible maximum levels stipulated by World Health Organization and the Brazilian Government.  相似文献   

16.
The primary objective of this study was to observe the evolution of anthropogenic radioactivity contamination in the Antarctic continent throughout the period 1997–1999. Moreover, results have been compared with those obtained for previous expeditions, starting from 1987. As far as 137Cs is concerned, interesting considerations could be made due to the great amount of available data. On the whole, radioactive contamination seems to be higher in continental than in marine environments. For lake algae, contamination seems to decrease gradually in the order: Tarn Flat, Edmondson Point, Carezza Lake. Focusing on 137Cs activity data, a clear temporal decreasing trend was observed in all samples: for sea water, values decreased from mean values of 0.9?Bq/m3 in 1987 to 0.5?Bq/m3 in 1999, a 56% decrease (20% of the total is due to natural decay of 137Cs). For lake waters and lake algae, the decreases are higher (80 and 30%, respectively) and the same can be assessed for sediments and soils, even if the resulting distributions are more complicated. The highest values for all radionuclides analysed were detected in terrestrial organisms (mosses, lake algae, and lichens). As a consequence, these matrices appear to be good bioindicators of radioactive contamination. Finally, although the Antarctic continent is affected by some degree by anthropogenic radioactive pollution, our results for 137Cs show that we are facing a progressive decrease. Moreover, contamination in other parts of the world is much higher: from 6–10 times in the Mediterranean Sea and 20–50 times in the North Sea and Black Sea.  相似文献   

17.
观察、比较正交信号校正(OSC)滤噪前后, 用不同的模式识别方法对正常成人血清代谢组1H NMR谱进行分析的效果, 以探讨NMR代谢组学技术应用于临床研究和疾病早期诊断的可行性. 78例正常成人在采血前按常规要求禁食8 h, 记录血清一维600 MHz氢谱后, 分别采用主成分分析(PCA)、偏最小二乘法-判别分析(PLS-DA)以及簇类的独立软模式法(SIMCA)对氢谱进行模式识别分析. 结果表明: 虽然采血前并无其它诸如饮食、生活方式、生理周期等方面的严格限制, 采用OSC 滤噪后, PLS-DA能够完全区分不同性别的血清氢谱, 其判别能力优于PCA和SIMCA. 而且采用OSC滤噪与文献报道的未经OSC处理的PLS-DA法获得的与性别分类有关的主要NMR积分区段基本相同. 从OSC去除不同数目的隐变量后所致的PLS-DA模型的性能改变可见: OSC去除两个隐变量时, 前两个隐变量的特征值明显比后面的大; 剩余残差为20.82%, 即去除了79.18%的X变量中与反应变量Y不相关的系统变异. 此时PLS-DA计算所得的隐变量个数为1; 而不使用OSC或用OSC去除一个隐变量时, PLS-DA所得的隐变量个数分别为3和2. 作为PLS-DA模型质量的评价指标, R2X表示PLS-DA模型计算所获得的隐变量反映自变量X的变异的百分比, R2Y则表示隐变量反映因变量Y的变异的百分比, Q2 (cum)为交叉验证后PLS-DA模型所获隐变量能够预测XY变异的累计百分比. R2X在OSC去除两个隐变量时达到最低值, 表明此时PLS-DA计算模型包含的系统变异最少; R2Y与Q2 (cum)都达到80%以上并趋于稳定, 说明OSC去除两个隐变量时PLS-DA模型的质量优良. 显然, OSC可去除饮食、环境等因素的影响, 降低临床样本的不均一性, 这对于NMR代谢组学技术应用于临床研究至关重要. OSC滤噪去除的隐变量个数应根据剩余残差、去除隐变量的特征值大小、PLS-DA模型计算所得的隐变量个数和反映模型质量的相关指标加以判断.  相似文献   

18.
The aim of this study was to determine whether multiple use cellulosic medical textiles (cotton blends, Tencel®) could provide protection against contamination after sterilization, regardless of the barrier system of only qualified materials, as per EN 868-2, used in the process. New methods for testing permeability and durability of the microbial barrier cellulosic textiles were developed. The most resistant endospores of two apathogenic bacteria of the Bacilllus genus (Geobacillus stearothermophilus and Bacillus atrophaeus) were used. Testing was conducted after 1, 10, 20, 30 and 50 washing and sterilization cycles under real hospital conditions of the University Hospital Centre Zagreb. The retention period of the microbial barrier of the diagonally packaged packages (one layer; EN ISO 11607-1:2009) after sterilization was tested after the time period of 1, 2 and 3 months of storage under controlled conditions. Bacterial permeability occurred in cellulosic medical textiles when they were contaminated with an extremely high quantity of aerobe bacterial spores. During the testing of microbial barrier durability, the package remained uncontaminated after 1, 2 and 3 months of storage. Medical cellulose textiles used under real hospital conditions functioned properly as a microbial barrier system after 50 cycles of washing and sterilization and 3 months of storage, as the sterilized content was not contaminated at all; they could be used as a microbe barrier system for packing in sterilization, regardless of the fact that they did not meet the standard EN 868-02:2009 Packaging materials for terminally sterilized medical devices. Part 2: sterilization wrap—requirements and test methods or the International standard, for example EN ISO 11607-1:2009 Packaging for terminally sterilized medical devices, part 1: requirements for materials, sterile barrier systems and packaging systems.  相似文献   

19.
Microcalorimetry was used to investigate the microbial activity in three types of soil (orchard soil, crop soil, forest soil) in Wuhan, China, and to evaluate the influence of different concentrations of lead (Pb2+) on soil microbial activity. The experimental results revealed that due to different physical and chemical characteristics of the soils, soil microbial activity in three soil samples were in a descending sequence: orchards soil, crops soil, forest soil. Six levels of Pb viz. 0, 10, 20, 40, 80, 160 μg·g−1 were applied in these soils, and the results showed that an increase of the amount of Pb2+ is associated with a decrease in microbial activity in the soils due to the toxic effect of Pb2+. In order to gain further insight of the sequential change of microorganisms, determination of colony forming units (CFU) was performed to provide a negative linear correlation between the heat effect and the respective number of microorganisms in the system.  相似文献   

20.
We demonstrate an improved method based on continuous‐flow elemental analyser pyrolysis isotopic ratio mass spectrometry (CF‐EA‐PY‐IRMS) to measure the 2H/1H ratios of water trapped in halite crystals. Two challenges to overcome are the low hydrogen concentration of samples (10‐50 μmol H2·g?1) and the high chloride concentration released when reacting halite in an elemental analyser. We describe an optimization procedure for determining the 2H/1H ratio of this trapped water with an acceptable accuracy. This technique involves the use of a high‐temperature Cr reactor to quantitatively convert H2O into H2. The initial step was performed on halite crystals precipitated from a water reservoir where 2H/1H ratios were monitored from its initial stage until the end of evaporation. The 2H/1H isotopic analyses were automated online in continuous‐flow mode. Precision of the method was determined for those “synthetic” samples with hydrogen concentrations ranging from 0.2 to 0.5 wt%. 2H/1H isotopic ratios of evaporating waters bracket the compositions of water inclusions. The formation of fluid inclusions is not instantaneous and records the isotopic signature of the residual waters across a time range during which the isotopic values of the water still evolve. This property explains why the δ2HVSMOW standard deviation of ±5‰ (2σ) observed for 10‐mg aliquots of halite exceeds the instrumental error (about ±1.5‰ 2σ) determined on the basis of IAEA‐CH7, NBS 30, and NBS 22 references along with calibrated waters with and without added halite crystals. We also applied this method to Mesoproterozoic (1.4 Ga) and Neoproterozoic (0.8 Ga) halite samples with relatively low hydrogen concentrations (300‐1500 ppm). The measured δ2HVSMOW values for Precambrian waters range from ?89‰ to ?54‰. We propose that this technique offers a new perspective and great potential for palaeoenvironmental reconstructions based on the 2H/1H analyses of water trapped in halite.  相似文献   

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