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1.
In this study, for the first time, an organic solvent-free air-assisted liquid–liquid microextraction method has been reported for the extraction and preconcentration of phthalic acids (o-phthalic acid, m-phthalic acid, and p-phthalic acid) from edible oil samples. The method is based on the repeated aspirating/injection of an alkaline aqueous solution and the oil sample mixture in a conical bottom centrifuge tube to form a cloudy solution. After phase separation by centrifuging, the sedimented phase is directly analyzed by high-performance liquid chromatography–diode array detection. Under the optimum extraction conditions, the method showed low limits of detection and quantification between 0.11–0.29 and 0.28–0.91 ng mL?1, respectively. Extraction recoveries and enrichment factors were from 81 to 97% and 406 to 489, respectively. The relative standard deviations for the analysis of 5 ng mL?1 of each analyte were less than 5.9% for intraday (n = 6) and interday (n = 5) precisions. Finally, different oil samples were successfully analyzed using the proposed method and m-phthalic acid, and p-phthalic acid were determined in some of them at ng mL?1 level.  相似文献   

2.
This paper reports the results of the experimental study of parameters for a DC oxygen discharge with water cathode in the pressure range of 0.1–1 bar and the discharge current of 40 mA. The radius of positive column, the cathode voltage drop, the cathode current density and the electric field strength were measured. Rotational temperatures of N2 (C3Πu, V = 0) and OH (A2Σ, V = 0) and absolute line intensities of atomic oxygen with wave length of 845 and 777 nm were determined as well. Plasma composition modeling was carried out by the combined solution of the Boltzmann equation for electrons, the equations of vibrational kinetics for ground states of N2, O2, H2O molecules, and the equations of chemical kinetics, and the plasma conductivity equation. Calculations were carried out taking into consideration the discharge radial heterogeneity and using experimental values of E/N and gas temperatures. The main particles being formed in plasma were shown to be ·OH, H2O2, O(3P), O2(a1Δg), O2(b1Σ g + ), H(1S). On the basis of this calculation and experimental values of line intensities, the populating mechanism of (3p 3P) level of atomic oxygen was discussed. The comparison of some properties of discharges in O2, N2 and air was done.  相似文献   

3.
Microbial-derived surfactants are molecules of great interest due to their environmentally friendly nature and low toxicity; however, their production cost is not competitive when compared to synthetics. Marine microorganisms are exposed to extremes of pressure, temperature, and salinity; hence, they can produce stable compounds under such conditions that are useful for industrial applications. A screening program to select marine bacteria able to produce biosurfactant using low-cost substrates (mineral oil, sucrose, soybean oil, and glycerol) was conducted. The selected bacterial strain showed potential to synthesize biosurfactants using mineral oil as carbon source and was identified as Brevibacterium luteolum. The surface-active compound reduced the surface tension of water to 27 mN m?1 and the interfacial tension (water/hexadecane) to 0.84 mN m?1 and showed a critical micelle concentration of 40 mg L?1. The biosurfactant was stable over a range of temperature, pH, and salt concentration and the emulsification index (E24) with different hydrocarbons ranging from 60 to 79 %. Structural characterization revealed that the biosurfactant has a lipopeptide nature. Sand washing removed 83 % of crude oil demonstrating the potential of the biosurfactants (BS) for bioremediation purposes. The new marine B. luteolum strain showed potential to produce high surface-active and stable molecule using a low-cost substrate.  相似文献   

4.
Novel apparatus for the generation of underwater plasma based on DC diaphragm discharge excited in a vapor bubble has been developed for decontamination and disinfection of conductive water. The apparatus allows deposition of relatively high applied power into the discharge (order of kW) and the treatment of a relatively large volume of liquid (order of L/min). The apparatus is operated at the quasi-pulse regime with self-terminating discharge pulses (with a repetition rate of 15–20 Hz) generated upon the formation of the vapor bubble inside the diaphragm (capillary) and its subsequent breakdown. The effects of input power, solution conductivity and the method of liquid flow through the reactor on the plasmachemical yield of H2O2 production and degradation of phenol have been determined. The biocidal effects of the apparatus were evaluated on inactivation of bacteria E. coli and E. faecalis suspended in aqueous NaCl solutions and on growth inhibition of the cyanobacterium Planktothrix sp. in natural lake water. The apparatus proved to be capable of efficiently reducing biological contamination in water, especially when operated in the plug-flow regime (up to a 5-log reduction in bacteria after 3 passes through the reactor). In the case of cyanobacteria, the growth inhibition further proceeded after exposure to the discharge and one pass of the biomass through the reactor was sufficient to reduce the algae in the water.  相似文献   

5.
Testosterone and testosterone enanthate are performance-enhancing substances that are banned in racehorses competing in the State of Pennsylvania (PA). A tolerance concentration of 2,000 pg mL?1 plasma has been established for testosterone in intact colts and stallions at the time they are competing in PA. Testosterone enanthate is a precursor of testosterone and can be used to boost plasma testosterone concentration above natural, age and seasonally variable plasma concentration. To control abuse, a verifiable method for rapid determination of both substances in equine plasma was needed. For this reason, an ultra high performance liquid chromatography-tandem mass spectrometry method for high-throughput analysis of both analytes in equine plasma was developed. Analytes were recovered from plasma by liquid–liquid extraction using mixture of methyl tert-butyl ether and ethyl acetate (50:50, v/v), separated on a C18 sub-2 μm column and detected on a triple quadrupole mass spectrometer using positive electrospray ionization mode with selected reaction monitoring scan. SRM ion transitions of m/z 289 → m/z 97, m/z 289 → m/z 109, m/z 289 → m/z 79 were used for testosterone identification while m/z 401 → m/z 253, m/z 401 → m/z 271, m/z 401 → m/z 97 were employed for testosterone enanthate. Retention time and product ion intensity ratio were used as confirmation criteria to ascertain the presence of both analytes in equine plasma. The limits of detection, quantification and confirmation were 50 pg 0.5 mL?1, 100 pg 0.5 mL?1 and 250 pg 0.5 mL?1, respectively for both analytes. The method was validated for recovery efficiency, sensitivity, matrix effect, linearity, precision and accuracy. This method is routinely used in the PA program for androgenic anabolic steroids doping control in racehorses and in the on-going testosterone enanthate pharmacokinetics study. The method is defensible, fast, selective, specific and reproducibly reliable.  相似文献   

6.
Montmorillonite-supported nanoscale zero-valent iron (M-nZVI) was synthesized by sodium borohydride reduction and characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and field emission scanning electron microscopy (FE-SEM). The interaction of uranium with M-nZVI was studied using batch technique under different experimental conditions such as pH, ionic strength, initial U(VI) concentration, solid-to-liquid ration (m/V), and temperature. The presence of montmorillonite decreased the aggregation while increased the specific surface area (SSA) of the iron nanoparticles. The SSA for as-synthesized M-nZVI was 91.42 m2/g, higher than 26.60 and 10.23 m2/g for nZVI and montmorillonite, respectively. The removal efficiency of U(VI) using M-nZVI was significantly affected by the pH of the aqueous solution, whereas it was slightly affected by ionic strength and temperature. The isoelectric point of M-nZVI was at pH 5.6; however the results indicated that the optimum removal efficiency of U(VI) using M-nZVI was achieved at a pH range 3.0–5.0. The experiments with aqueous solution containing 100 μg/L of U(VI) showed that the removal efficiency of the as-synthesized M-nZVI was about 978 μg/g at pH 3.0. These results show that M-nZVI has a potential as a novel material for removing U(VI) from aqueous solution.  相似文献   

7.
Plasma–liquid interaction has already been a hotspot in the research field of plasma medicine. Aqueous reactive oxygen species (ROS) generated in this process are widely accepted playing a crucial role in plasma biomedical effects. In this paper, chemistry pathways among various aqueous ROS induced by He + O2 plasmas are investigated by a numerical model. Simulation results show that these aqueous ROS can be classified into two groups according to their production ways: the group of species including O, 1O2 and e directly produced in plasma, and the other group of species including O2 ?, H2O2, O3, etc. produced by liquid reactions. A key reaction chain of e → O2 ? → HO2(→ HO2 ?) → H2O2 is found to be important in the plasma-induced liquid chemistry. Furthermore, impacts of changes in plasma and solution conditions on aqueous ROS concentrations are studied as well. It is found that changes in plasma conditions (O2 ratio in the discharge gas/power density) can globally influence the concentrations of almost every aqueous ROS, while conditions changes of the treated liquid (pH/dissolved oxygen) only partially influence the concentrations of some specific species including O2 ?/HO2, O3 ?/HO3 and H2O2. The revelations of the liquid chemistry pathways and the dependence of ROS dosage on the treatment conditions offer a better understanding on the plasma–liquid interactions, as well as provide optimized dosage control approaches for biomedical applications.  相似文献   

8.
Ceragenins/cationic steroid antimicrobials (CSAs) are a group of cholic acid derivatives with many properties that make them favourable for application as anti-infective agents. CSA-107 is also a member of this group that was labelled with 99mTc by using SnCl2·2H2O as reducing agent and Na–K tartrate as transchelating agent. Labelling efficiency was optimized by varying the amount of reducing agent, pH, and time of incubation. Labelling efficiency and the stability of 99mTc-CSA-107 in human serum was determined by paper and thin layer chromatography, which were >95 and >90 % respectively. In vitro binding of 99mTc-CSA-107 was >95 % determined by using Staphylococcus aureus bacteria.  相似文献   

9.
Column experiments were utilized to investigate the effects of nitrate injection on sulfate-reducing bacteria (SRB) inhibition and microbial enhanced oil recovery (MEOR). An indigenous microbial consortium collected from the produced water of a Brazilian offshore field was used as inoculum. The presence of 150 mg/L volatile fatty acids (VFA´s) in the injection water contributed to a high biological electron acceptors demand and the establishment of anaerobic sulfate-reducing conditions. Continuous injection of nitrate (up to 25 mg/L) for 90 days did not inhibit souring. Contrariwise, in nitrogen-limiting conditions, the addition of nitrate stimulated the proliferation of δ-Proteobacteria (including SRB) and the associated sulfide concentration. Denitrification-specific nirK or nirS genes were not detected. A sharp decrease in water interfacial tension (from 20.8 to 14.5 mN/m) observed concomitantly with nitrate consumption and increased oil recovery (4.3 % v/v) demonstrated the benefits of nitrate injection on MEOR. Overall, the results support the notion that the addition of nitrate, at this particular oil reservoir, can benefit MEOR by stimulating the proliferation of fortuitous biosurfactant-producing bacteria. Higher nitrate concentrations exceeding the stoichiometric volatile fatty acid (VFA) biodegradation demands and/or the use of alternative biogenic souring control strategies may be necessary to warrant effective SRB inhibition down gradient from the injection wells.  相似文献   

10.
Recently ultrasmall superparamagnetic iron oxide (USPIO) nanoparticles (NPs) have been widely used for medical applications. One of their important applications is using these particles as MRI contrast agent. While various research works have been done about MRI application of USPIOs, there is limited research about their uptakes in various organs. The aim of this study was to evaluate the biodistribution of dextran coated iron oxide NPs labelled with 99mTc in various organs via intravenous injection in Balb/c mice. The magnetite NPs were dispersed in phosphate buffered saline and SnCl2 which was used as a reduction reagent. Subsequently, the radioisotope 99mTc was mixed directly into the reaction solution. The labeling efficiency of USPIOs labeled with 99mTc, was above 99 %. Sixty mice were sacrificed at 12 different time points (From 1 min to 48 h post injections; five mice at each time). The percentage of injected dose per gram of each organ was measured by direct counting for 19 harvested organs of the mice. The biodistribution of 99mTc-USPIO in Balb/c mice showed dramatic uptake in reticuloendothelial system. Accordingly, about 75 percent of injected dose was found in spleen and liver at 15 min post injection. More than 24 % of the NPs remain in liver after 48 h post-injection and their clearance is so fast in other organs. The results suggest that USPIOs as characterized in our study can be potentially used as contrast agent in MR Imaging, distributing reticuloendothelial system specially spleen and liver.  相似文献   

11.
Methoxetamine is a new ketamine derivative designer drug which has recently become available via the Internet marketed as “legal ketamine”. It is a new dissociative recreational drug, acting as an NMDA receptor antagonist and dopamine reuptake inhibitor. The objective of this study was to develop on-line automated sample preparation using a TurboFlow device coupled with liquid chromatography with ion-trap mass spectrometric detection for measurement of methoxetamine in human plasma. Samples (100 μL) were vortex mixed with internal standard solution (ketamine-d4 in acetonitrile). After centrifugation, 20 μL of the supernatant was injected on to a 50 mm?×?0.5-mm C18XL Turboflow column. The retained analytes were then back-flushed on to a 50 mm?×?3-mm (3 μm) Hypersil Gold analytical column for chromatographic separation, then eluted with a formate buffer–acetonitrile gradient. Methoxetamine and the IS were ionized by electrospray in positive mode. Parent [M + H]+ ions were m/z 248.1 for methoxetamine and m/z 242.0 for the IS. The most intense product ions from methoxetamine (m/z 203.0) and the IS (m/z 224.0) were used for quantification. The assay was accurate (96.8–108.8 % range) and precise (intra and inter-day coefficients of variation <8.8 %) over the range of 2.0 (lower limit of quantification) to 1000.0 ng mL?1 (upper limit of quantification). No matrix effect was observed. This method has been successfully applied to determination of plasma concentrations of methoxetamine in the first French hospitalization case report after acute intoxication; the plasma concentration was 136 ng mL?1.  相似文献   

12.
NADP+-dependent isocitrate dehydrogenase from Yarrowia lipolytica CLIB122 (YlIDP) was overexpressed and purified. The molecular mass of YlIDP was estimated to be about 81.3 kDa, suggesting its homodimeric structure in solution. YlIDP was divalent cation dependent and Mg2+ was found to be the most favorable cofactor. The purified recombinant YlIDP displayed maximal activity at 55 °C and its optimal pH for catalysis was found to be around 8.5. Heat inactivation studies revealed that the recombinant YlIDP was stable below 45 °C, but its activity dropped quickly above this temperature. YlIDP was absolutely dependent on NADP+ and no NAD-dependent activity could be detected. The K m values displayed for NADP+ and isocitrate were 59 and 31 μM (Mg2+), 120 μM and 58 μM (Mn2+), respectively. Mutant enzymes were constructed to tentatively alter the coenzyme specificity of YlIDP. The K m values for NADP+ of R322D mutant was 2,410 μM, being about 41-fold higher than that of wild type enzyme. NAD+-dependent activity was detected for R322D mutant and the K m and k cat values for NAD+ were 47,000 μM and 0.38 s?1, respectively. Although the R322D mutant showed low activity with NAD+, it revealed the feasibility of engineering an eukaryotic IDP to a NAD+-dependent one.  相似文献   

13.
A rapid and sensitive liquid chromatographic–tandem mass spectrometric method has been developed and validated for the estimation of sarpogrelate in human plasma. Sarpogrelate was extracted from human plasma by solid-phase extraction. Temocapril was used as the internal standard. Heated electron spray ionization mass spectrometry was performed on a TSQ Quantum Ultra MS system. The LC column was a Hypurity C18 and the mobile phase was 2 mM ammonium formate (pH 3.00 ± 0.05):acetonitrile (30:70 v/v). A flow rate of 0.250 mL min?1 was used. The quantitative analyses were carried out in the positive ion and full scan mode over the mass range m/z 60–500. The capillary, vaporiser temperatures were 325 and 200 °C respectively. The sheath gas pressure, spray voltage, collision energy and tube lense were 40, 3,500 V, 19 V, 198 V, respectively, and the mass spectra of the drugs were recorded by total ion monitoring. Retention times and characteristic mass fragments were recorded and the chosen diagnostic mass fragments were monitored in the mass chromatography mode. Signal intensities of each of the mass fragments: m/z 477 [M + H]+ for temocapril, m/z 430 [M + H]+ for sarpogrelate, were used for quantification. The calibration curves (the ratio between the peak areas as signal intensities of the drug analyzed and that of the internal standard (temocapril: m/z 477 [M + H]+) vs. the concentration of drug) exhibited linearity over the concentration range 5.00–2,500.00 ng mL?1 human plasma. The recovery and the accuracy were calculated by comparing the peak areas as the signal intensities of each mass fragment for the drug in spiked samples after solid-phase extraction from human plasma to the peak area as the signal intensity of the mass fragment of internal standard sample. The method involves a rapid solid phase extraction from plasma, simple isocratic chromatography conditions and mass spectrometric detection that enables detection up to picogram levels with a total run time of 3.0 min only. The method was validated over the range of 5.0–2,500.0 ng mL?1. The absolute recoveries for sarpogrelate (93.72%) and IS (91.42%) achieved from spiked plasma samples were consistent and reproducible.  相似文献   

14.
A sensitive and selective liquid chromatography?Ctandem mass spectrometry method for the determination of pethidine and atropine in rabbit plasma was developed and validated. The analytes and internal standard (IS) are extracted from plasma by liquid?Cliquid extraction using ethyl acetate, and separated on a Zorbax SB-Aq column (2.1 × 150 mm, 3.5 ??m) using acetonitrile?C0.1% formic acid as mobile phase with gradient elution. Electrospray ionization source was applied and operated in positive ion mode, and multiple reaction monitoring mode was used for quantification using target fragment ions m/z 247.8 ?? 219.7 for pethidine, m/z 289.9 ?? 123.8 for atropine and m/z 295.0 ?? 266.8 for IS, respectively. The assay is linear over the range of 5?C1,000 ng mL?1 for pethidine and atropine, with a lower limit of quantification of 3 ng mL?1 for pethidine and 5 ng mL?1 for atropine. Intra-day and inter-day precision are less than 11% and the accuracy are in the range of 90.4?C106.3%. Furthermore, the newly developed method is successfully used for the determination of pethidine and atropine in rabbit plasma for pharmacokinetic study.  相似文献   

15.
《Analytical letters》2012,45(3):452-460
A corona discharge (CD) ionization source was prepared for a planar high-field asymmetric waveform ion mobility spectrometer (FAIMS). The effects of discharge current and discharge distance on ionization efficiency were investigated; and the electric field dependence of the ion injection in the reaction region was studied. The results showed that the discharge current of CD source had good linearity with the intensity of reactant ion peak (RIP), and the RIP intensity increased to a stable level at the discharge distance of >5 mm. An injection electrode was introduced to improve the ionization efficiency. A square-wave voltage applied to the electrode was found to provide optimal performance of ion injection and utilization. The operating parameters of the CD-FAIMS were optimized to achieve trace level detection of dimethyl methylphosphonate (DMMP) sample. The detection limit for DMMP was 0.5 µg/m3.  相似文献   

16.
Saccharomyces cerevisiae PTCC5269 growth was evaluated to specify an optimum culture medium to reach the highest protein production. Experiment design was conducted using a fraction of the full factorial methodology, and signal to noise ratio was used for results analysis. Maximum cell of 8.84 log (CFU/mL) was resulted using optimized culture composed of 0.3, 0.15, 1, and 50 g L?1 of ammonium sulfate, iron sulfate, glycine, and glucose, respectively at 300 rpm and 35 °C. Glycine concentration (39.32 % contribution) and glucose concentration (36.15 % contribution) were determined as the most effective factors on the biomass production, while Saccharomyces cerevisiae growth had showed the least dependence on ammonium sulfate (5.2 % contribution) and iron sulfate (19.28 % contribution). The most interaction was diagnosed between ammonium sulfate and iron sulfate concentrations with interaction severity index of 50.71 %, while the less one recorded for glycine and glucose concentration was equal to 8.12 %. An acceptable consistency of 84.26 % was obtained between optimum theoretical cell numbers determined by software of 8.91 log (CFU/mL), and experimentally measured one at optimal condition confirms the suitability of the applied method. High protein content of 44.6 % using optimum culture suggests that Saccharomyces cerevisiae is a good commercial case for single cell protein production.  相似文献   

17.
Current gas ionization discharge techniques used in the removal of NOx from waste gases require large plasma sources, have high energy consumption, and may feature low NOx removal rates. We develop a system to generate reactive oxygen species through a strong ionization discharge, which is injected into a flow of simulated waste gas. The relative proportions and temperatures of input gases were controlled and the rate of consumption by reactive species was monitored. HNO3 oxidization products of NOx were also collected and measured. The molar ratio of reactive oxygen species to NO was optimized to improve the rate of NOx removal. A input gas temperature of 58–60 °C was also found to be optimal. The O2 volume fraction has almost no influence on NOx removal, while H2O volume fractions above 6 %, gave rise to NOx removal rates of 97.2 %. The present study addresses disadvantages of current gas ionization discharge and requires no catalyst, reducing agent or oxidant.  相似文献   

18.
A multi-needle-to-plate pulsed discharge plasma reactor was designed to investigate its potential for polyvinyl alcohol-containing wastewater (PVA) treatment. The effects of some operational parameters such as PVA initial concentration, pulse peak discharge voltage, air flow rate, solution pH value, and iron additives on PVA degradation were examined. The results indicated that PVA could be effectively degraded from aqueous solutions. PVA degradation efficiency was 76.0 % within 60 min’s discharge plasma treatment with 1.5 mmol L?1 Fe2+ addition. Decreasing PVA initial concentration and increasing pulse peak discharge voltage were both beneficial for PVA degradation. There existed appropriate air flow rate for obtaining great PVA degradation efficiency in the present study. A little acid environment was conducive to PVA degradation. The presence of Fe2+ and Cu2+ could both benefit PVA degradation, and the increment of Fe2+ and Cu2+ concentrations to a certain extent could enhance its degradation efficiency, as well as energy yield. PVA possible degradation mechanisms were discussed, and the degradation processes were mainly triggered by the reactions of PVA with \(^{ \cdot } {\text{OH}}\) radicals.  相似文献   

19.
The Fe2O3/lignite semi-coke sorbent was prepared by co-precipitation method with assistance of ultrasonic irradiation and underwent 4 sulfidation–regeneration cycles with O2/N2 as regeneration gases. The fresh, sulfided, and regenerated sorbents were characterized using XRD, SEM, XPS, and BET technologies in this paper. The regeneration mechanism was also discussed. It was found that in the oxygen atmosphere, FeS in the sulfided sorbent reacted with oxygen to produce Fe2O3 and SO2, the sulfate formed in regeneration process is easy to decompose at higher temperature. Regeneration kinetic studies were also performed at regeneration temperatures of 625–700 °C. It was found that the reaction order of regeneration with respect to O2 is first order. The equivalent grain model can be effectively used to correlate with the experimental data. In the early stage of reaction (x < 65 %), the regeneration is controlled by the chemical reaction, while it is controlled by the diffusion through the product layer in the latter stage (x > 70 %). According to the model, the apparent activation energy and the corresponding frequency factor for two different stages are 14.73 kJ mol?1 and 4.43 × 10?2 m s?1, 31.32 kJ mol?1 and 5.77 × 10?4 m2 s?1, respectively.  相似文献   

20.
A ligand of N-2-(furylmethyl iminodiacetic acid) (FMIDA) has been easily labeled by a tetradentate chelating agent of [99mTc]. Factors like a stannous chloride solution as a reducing agent (100 μg), substrate amount (100 μg), pH (7), in vitro stability (8 h) and temperature (37 °C) have been systematically studied to optimize high radiochemical yield (98.0%). The radiochemical conversion was calculated on thin-layer chromatography, paper electrophoresis, and high performance liquid chromatography. Biodistribution study showed that this complex was removed from the kidneys and bladder path way during 1 h post injection. Therefore, [99mTc]FMIDA may be used as renal function radiotracer.  相似文献   

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