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1.
A new and simple method has been proposed to prepare magnetic Fe3O4-chitosan (CS) nanoparticles by cross-linking with sodium tripolyphosphate (TPP), precipitation with NaOH and oxidation with O2 in hydrochloric acid aqueous phase containing CS and Fe(OH)2, and these magnetic CS nanoparticles were used to immobilize lipase. The effects on the sequence of adding NaOH and TPP, the reaction temperature, and the ratio of CS/Fe(OH)2 were studied. TEM showed that the diameter of composite nanoparticles was about 80 nm, and that the magnetic Fe3O4 nanoparticles with a diameter of 20 nm were evenly dispersed in the CS materials. Magnetic measurement revealed that the saturated magnetisation of the Fe3O4-CS nanoparticles could reach 35.54 emu/g. The adsorption capacity of lipase onto nanoparticles could reach 129 mg/g; and the maximal enzyme activity was 20.02 μmol min−1 mg−1 (protein), and activity retention was as high as 55.6% at a certain loading amount.  相似文献   

2.
Nano-sized crystals of maghemite iron oxide (γ-Fe2O3) were synthesized onto the surface of NaY-zeolite crystals by immobilizing a polynuclear iron complex [Fe4O2(O2CCH3)7(bpy)2](ClO4) (bpy = 2,2′-bipyridine) and subsequent calcination of the material in oxygen. Superparamagnetic γ-Fe2O3 particles with sizes ∼5 nm were formed on the surface of the zeolite matrix. The nano-composite, γ-Fe2O3@NaY has been subsequently subjected for thorough characterization with several spectroscopic techniques as well as magnetic and transmission electron microscopic measurements. This confirms the formation of maghemite nanoparticles on a NaY-zeolite surface. γ-Fe2O3@NaY shows a remarkable catalytic efficiency in epoxidation reactions with various olefins using tert-BuOOH as oxidant. Notably, styrene shows a remarkable high conversion (90%) as well as epoxide selectivity (95%) while trans-stilbene is completely converted to its oxide with tert-BuOOH over a γ-Fe2O3@NaY catalyst.  相似文献   

3.
Magnetic Fe3O4-chitosan nanoparticles are prepared by the coagulation of an aqueous solution of chitosan with Fe3O4 nanoparticles. The characterization of Fe3O4-chitosan is analyzed by FTIR, FESEM, and SQUID magnetometry. The Fe3O4-chitosan nanoparticles are used for the covalent immobilization of lipase from Candida rugosa using N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide (EDC) and N-hydroxysuccinimide (NHS) as coupling agents. The response surface methodology (RSM) was employed to search the optimal immobilization conditions and understand the significance of the factors affecting the immobilized lipase activity. Based on the ridge max analysis, the optimum immobilization conditions were immobilization time 2.14 h, pH 6.37, and enzyme/support ratio 0.73 (w/w); the highest activity obtained was 20 U/g Fe3O4-chitosan. After twenty repeated uses, the immobilized lipase retains over 83% of its original activity. The immobilized lipase shows better operational stability, including wider thermal and pH ranges, and remains stable after 13 days of storage at 25 °C.  相似文献   

4.
Electrically active magnetic nanocomposites (EAMNCs), Au nanoparticles/self-doped polyaniline@Fe3O4 (AuNPs/SPAN@Fe3O4) with well-defined core/shell structure, were first synthesized by a simple method. The morphology and composition of the as-synthesized AuNPs/SPAN@Fe3O4 nanocomposite have been characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared (FT–IR), ultraviolet–visible (UV–Vis), X-ray powder diffraction (XRD), and thermogravimetric analysis (TGA). Horseradish peroxidase (HRP)–AuNPs/SPAN@Fe3O4 biocomposites were immobilized onto the surface of indium tin oxide (ITO) electrode to construct an amperometric hydrogen peroxide (H2O2) biosensor. The effects of HRP dosage, solution pH, and the working potential on the current response toward H2O2 reduction were optimized to obtain the maximal sensitivity. Under the optimal conditions, the proposed biosensor exhibited a linear calibration response in the range of 0.05 to 0.35 mM and 0.35 to 1.85 mM, with a detection limit of 0.01 mM (signal-to-noise ratio = 3). The modified electrode could virtually eliminate the interference of ascorbic acid (AA) and uric acid (UA) during the detection of H2O2. Furthermore, the biosensor was applied to detect H2O2 concentration in real samples, which showed acceptable accuracy with the traditional potassium permanganate titration.  相似文献   

5.
The simple preparation of Co3O4 nanoparticles from a solid organometallic molecular precursor N-N′-bis(salicylaldehyde)-1,2-phenylenediimino cobalt(II); Co(salophen) has been achieved via two simple steps: firstly, the Co(salophen) precursor was precipitated from the reaction of cobalt(II) acetate and N-N′-bis(salicylaldehyde)-1,2-phenylenediimino; H2salophen; in propanol under nitrogen condition; then, cubic phase Co3O4 nanoparticles with the size of mostly 30-50 nm could be produced by thermal treatment of the Co(salophen) in air at 773 K for 5 h. The as-synthesized products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and scanning electronic microscopy (SEM). These results confirm that the resulting oxide was pure single-crystalline Co3O4 nanoparticles. The optical property test indicates that the absorption peak of the nanoparticles shifts towards short wavelength, and the blue shift phenomenon might be ascribed to the quantum effect. The hysteresis loops of the obtained samples reveal the ferromagnetic behaviors the enhanced coercivity (Hc) and decreased saturation magnetization (Ms) in contrast to their respective bulk materials.  相似文献   

6.
Supercritical water gasification (SCWG) of glucose solution (50-200 g/L), a simulated aqueous organic waste (composed of glucose, acetic acid and guaiacol) and a real aqueous organic waste stream generated from a sludge hydrothermal liquefaction process was performed in a bench-scale continuous down-flow tubular reactor with novel 0.1RuNi/γ-Al2O3 or 0.1RuNi/activated carbon (AC) catalyst (10 wt.% Ni with a Ru-to-Ni molar ratio of 0.1). 0.1RuNi/γ-Al2O3 was very effective in catalyzing SCWG of glucose solution and the simulated aqueous organic waste, attaining an H2 yield of 53.9 mol/kg dried feedstock at 750 °C, 24 MPa and a WHSV of 6 h−1. However, the γ-Al2O3-supported catalyst was not resistant to the attack of alkali and nitrogen compounds in the real waste during the SCWG of the real aqueous organic waste, whereas the AC-based catalyst exhibited higher stability. This research provides a promising approach to the treatment and valorization of aqueous organic waste via SCWG.  相似文献   

7.
Powdered Fe2O3-Fe2(MoO4)3 with different amounts of iron and molybdate precursors was prepared by a solvothermal route, followed by a supercritical drying and oxidation at 500 °C. The possibility to arrange Fe or Mo precursors in excess into a methanol solution makes one accessible to the preparation of iron(III) molybdate samples with different composition. The structural parameters and relationship between different phases in the composition are obtained from Rietveld profile refinement. Our intention was to modify the magnetic properties of Fe2(MoO4)3 by adding the crystalline phase of Fe2O3, which carries a Fe-O magnetic component. A possible contribution to the magnetization and the magnetic susceptibility by this magnetic component is analyzed in the temperature range 2-300 K. The observed higher magnetic susceptibilities are compared to those reported.  相似文献   

8.
In the present research, we report a greener, faster, and low-cost synthesis of gold-coated iron oxide nanoparticles (Fe3O4/Au-NPs) by different ratios (1:1, 2:1, and 3:1 molar ratio) of iron oxide and gold with natural honey (0.5% w/v) under hydrothermal conditions for 20 minutes. Honey was used as the reducing and stabilizing agent, respectively. The nanoparticles were characterized by X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscope (FESEM), energy-dispersive X-ray spectroscopy (EDXS), transmission electron microscopy (TEM), selected area electron diffraction (SAED), vibrating sample magnetometer (VSM), and fourier transformed infrared spectroscopy (FT-IR). The XRD analysis indicated the presence of Fe3O4/Au-NPs, while the TEM images showed the formation of Fe3O4/Au-NPs with diameter range between 3.49 nm and 4.11 nm. The VSM study demonstrated that the magnetic properties were decreased in the Fe3O4/Au-NPs compared with the Fe3O4-NPs. The cytotoxicity threshold of Fe3O4/Au-NPs in the WEHI164 cells was determined by using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. It was demonstrated no significant toxicity in higher concentration up to 140.0 ppm which can become the main candidates for biological and biomedical applications, such as drug delivery.  相似文献   

9.
Fe3O4 magnetic nanoparticles with different particle sizes were synthesized using two methods, i.e., a co-precipitation process and a polyol process, respectively. The atomic pair distribution analyses from the high-energy X-ray scattering data and TEM observations show that the two kinds of nanoparticles have different sizes and structural distortions. An average particle size of 6–8 nm with a narrow size distribution was observed for the nanoparticles prepared with the co-precipitation method. Magnetic measurements show that those particles are in ferromagnetic state with a saturation magnetization of 74.3 emu g−1. For the particles synthesized with the polyol process, a mean diameter of 18–35 nm was observed with a saturation magnetization of 78.2 emu g−1. Although both kinds of nanoparticles are well crystallized, an obviously higher structural distortion is evidenced for the co-precipitation processed nanoparticles. The synthesized Fe3O4 particles with different mean particle size were used for treating the wastewater contaminated with the metal ions, such as Ni(II), Cu(II), Cd(II) and Cr(VI). It is found that the adsorption capacity of Fe3O4 particles increased with decreasing the particle size or increasing the surface area. While the particle size was decreased to 8 nm, the Fe3O4 particles can absorb almost all of the above-mentioned metal ions in the contaminated water with the adsorption capacity of 34.93 mg/g, which is ∼7 times higher than that using the coarse particles. We attribute the extremely high adsorption capacity to the highly-distorted surface.  相似文献   

10.
Germanium tetra(tertiary butoxide), [Ge(OtBu)4], has been prepared by the reaction of GeCl4 with KOBut in benzene. It is a monomeric crystalline solid having a distorted tetrahedral configuration, defined by the coordination of four OBut groups around germanium atom. The TG analysis showed that the compound is thermally stable and volatilizes at around 130 °C. Europium doped and un-doped germanium oxide nanoparticles were prepared based on the urea hydrolysis of Ge(OtBu)4/Eu(OOCCH3)3 in ethylene glycol medium at 150 °C followed by heating the resulting product at 750 °C. The nanoparticles were characterized by XRD, TEM and PL measurements. The europium doped nanoparticles, which were nearly monodispersed (∼30 nm), showed luminescence and the Eu3+ ions were occupying the surface of the GeO2 nanoparticles.  相似文献   

11.
In situ cell separation and immobilization of bacterial cells for biodesulfurization were developed by using superparamagnetic Fe3O4 nanoparticles (NPs). The Fe3O4 NPs were synthesized by coprecipitation followed by modification with ammonium oleate. The surface-modified NPs were monodispersed and the particle size was about 13 nm with 50.8 emu/g saturation magnetization. After adding the magnetic fluids to the culture broth, Rhodococcus erythropolis LSSE8-1 cells were immobilized by adsorption and then separated with an externally magnetic field. The maximum amount of cell mass adsorbed was about 530 g dry cell weight/g particles to LSSE8-1 cells. Analysis showed that the nanoparticles were strongly absorbed to the surface and coated the cells. Compared to free cells, the coated cells not only had the same desulfurizing activity but could also be easily separated from fermentation broth by magnetic force. Based on the adsorption isotherms and Zeta potential analysis, it was believed that oleate-modified Fe3O4 NPs adsorbed bacterial cells mainly because of the nano-size effect and hydrophobic interaction.  相似文献   

12.
An electrochemical immunosensor for quantitative detection of α-fetoprotein (AFP) in human serum was developed using graphene sheets (GS) and thionine (TH) as electrode materials and mesoporous silica nanoparticles (MSNs) loaded with ferroferric oxide (Fe3O4) nanoparticles and horseradish peroxidase (HRP) as labels for signal amplification. In this study, the compound of GS and TH (GS–TH) was used as a substrate for promoting electron transfer and immobilization of primary antibody of AFP (Ab1). MSNs were used as a carrier for immobilization of secondary antibody of AFP (Ab2), Fe3O4, and HRP. The synergistic effect occurred between Fe3O4 and HRP and greatly improved the sensitivity of the immunosensor. This method could detect AFP over a wide concentration range from 0.01 to 25 ng ml−1 with a detection limit of 4 pg ml−1. This strategy may find wide potential application in clinical analysis or detection of other tumor markers.  相似文献   

13.
Microbial cells of Pseudomonas delafieldii were coated with magnetic Fe3O4 nanoparticles and then immobilized by external application of a magnetic field. Magnetic Fe3O4 nanoparticles were synthesized by a coprecipitation method followed by modification with ammonium oleate. The surface-modified Fe3O4 nanoparticles were monodispersed in an aqueous solution and did not precipitate in over 18 months. Using transmission electron microscopy (TEM), the average size of the magnetic particles was found to be in the range from 10 to 15 nm. TEM cross section analysis of the cells showed further that the Fe3O4 nanoparticles were for the most part strongly absorbed by the surfaces of the cells and coated the cells. The coated cells had distinct superparamagnetic properties. The magnetization (δs) was 8.39 emu · g−1. The coated cells not only had the same desulfurizing activity as free cells but could also be reused more than five times. Compared to cells immobilized on Celite, the cells coated with Fe3O4 nanoparticles had greater desulfurizing activity and operational stability.  相似文献   

14.
A novel amperometric biosensor for xanthine was developed based on covalent immobilization of crude xanthine oxidase (XOD) extracted from bovine milk onto a hybrid nanocomposite film via glutaraldehyde. Toward the preparation of the film, a stable colloids solution of core–shell Fe3O4/polyaniline nanoparticles (PANI/Fe3O4 NPs) was dispersed in solution containing chitosan (CHT) and H2PtCl6 and electrodeposited over the surface of a carbon paste electrode (CPE) in one step. Scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectrophotometry, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) were used for characterization of the electrode surface. The developed biosensor (XOD/CHT/Pt NPs/PANI/Fe3O4/CPE) was employed for determination of xanthine based on amperometric detection of hydrogen peroxide (H2O2) reduction at –0.35 V (vs. Ag/AgCl). The biosensor exhibited a fast response time to xanthine within 8 s and a linear working concentration range from 0.2 to 36.0 μM (R2 = 0.997) with a detection limit of 0.1 μM (signal/noise [S/N] = 3). The sensitivity of the biosensor was 13.58 μA μM−1 cm−2. The apparent Michaelis–Menten (Km) value for xanthine was found to be 4.7 μM. The fabricated biosensor was successfully applied for measurement of fish and chicken meat freshness, which was in agreement with the standard method at the 95% confidence level.  相似文献   

15.
1:2, 1:1, 3:2 and 6:2 AgX:L adducts (where L is a tridentate phosphine, in detail: 1,1,1-tris(diphenylphosphinomethyl)ethane (Me-triphos) and bis(2-diphenylphosphinoethyl)phenylphosphine (Ph-triphos), X = O3SCF3, O3SCH3, BF4 or O2CCF3) have been synthesized and characterized by IR, NMR (1H, 31P and 19F) and ESI MS spectroscopy. The stoichiometry of the complexes is strongly dependent on the ligand to metal ratio employed and also on the nature of the counterion. 31P NMR (solution) data also show the complexes existing in solution, in some cases, however, disproportionating to adducts of different nuclearity. Oligonuclear species have been detected through ESI MS spectroscopy that has been demonstrated as a powerful tool for the identification of the solution species. AgBF4:Me-triphos (1:2) has been structurally characterized as [Ag(P,P′-Me-triphos)2](BF4) · H2O · 7/2 MeOH, while Ag(O3SCF3): Ph-triphos: H2O (6:2:4) is a spectacular two-dimensional polymer.  相似文献   

16.
In this study, we present in vitro cytotoxicity of iron oxide (Fe3O4) and manganese oxide (MnO) using live/dead cell assay, lactate dehydrogenase assay, and reactive oxygen species detection with variation of the concentration of nanoparticles (5–500 μg/ml), incubation time (18–96 h), and different human cell lines (lung adenocarcinoma, breast cancer cells, and glioblastoma cells). The surface of nanoparticles is modified with polyethyleneglycol-derivatized phospholipid to enhance the biocompatibility, water-solubility, and stability under an aqueous media. While the cytotoxic effect was negligible for 18 h incubation even at highest concentration of 500 μg/ml, MnO nanoparticle represented higher level of toxicity than those of Fe3O4 and the commercial medical contrast reagent, Feridex after 2 and 4 day incubation time. However, the cytotoxicity of Fe3O4 is equivalent or better than Feridex based on the live/dead cell viability assay. The engineered MnO and Fe3O4 exhibited excellent stability compared with Feridex for a prolonged incubation time.  相似文献   

17.
Two dimeric head-on complexes of yttrium containing silico- and germanotungstate were isolated from the one-pot reaction of Y(NO3)3·6H2O with the lacunary Na10[MW9O34]·16H2O (M = Si and Ge) building blocks in an acetate buffer at pH 4.5. Both polyanions were structurally characterized using various solid-state analytics, such as single-crystal X-ray diffraction, single-crystal X-ray analysis shows that both polyanions crystallize in the monoclinic crystal system (S.G. P21/c). FT-IR spectroscopy, or thermogravimetric analysis. The stability of the polyanion in aqueous solution was studied by multinuclear NMR spectroscopy (183W, 89Y, 29Si, 13C, and 1H). As expected, the 183W NMR spectra display six peaks in the intensity ratio of 4:4:2:4:4:4 which indicates that both polyanions exist as dimeric entities in aqueous solution.  相似文献   

18.
The aqueous reaction of TiCl4 with citric acid at pH ∼ 4 (KOH), led to the surprising isolation of a species assembly K3[Ti(C6H6O7)2(C6H5O7)] · K4[Ti(C6H5O7)2(C6H6O7)] · 10H2O (1). The same system at pH ∼ 3 (neocuproine), led to the crystalline material (C14H13N2)2[Ti(C6H6O7)3] · 5H2O (2), while at pH 5.0 (NaOH), afforded Na3[Ti(C6H6O7)2(C6H5O7)] · 9H2O (3). Analytical, spectroscopic and structural characterization of 1, 2 and 3 revealed their distinct nature exemplified by mononuclear complexes bearing variably deprotonated citrates bound to Ti(IV). Solid-state 13C MAS NMR spectroscopy in concert with solution 13C and 1H NMR on 3 provided ample evidence for the existence of bound citrates of distinct coordination mode to the metal ion. Cyclic voltammetry defined the electrochemical signature of complex 2, thereby projecting the physicochemical profile of the species formulated by the aforementioned properties. Comparison of cyclic voltammetric data on available discrete Ti(IV)-citrate species depicts the electrochemical profile and an E1/2 value trend of the species in that binary system’s aqueous speciation, further substantiating the redox behavior of mononuclear Ti(IV)-citrate species in a pH-sensitive fashion. Collectively, the well-defined discrete species in 1-3 reflect and corroborate a synthetically challenging yet complex pH-specific picture of the aqueous Ti(IV) chemistry with the physiological citric acid, and shed light on the pH-dependent speciation in the binary Ti(IV)-citrate system.  相似文献   

19.
Five new octahedral iron(II) complexes [FeL2(4-dpa)]n(EtOH) (1), [FeL2(bipy)]n(DMF) (2), [FeL1(bpee)]n (3), [Fe2L3(1-meim)4](1-meim)4 (4) and [FeL1(DMAP)2] (5), with L1 and L2 being tetradentate coordinating Schiff base like ligands (L1 = (E,E)-[{diethyl-2,2′-[1,2-phenylenebis(iminomethylidyne)]bis[3-oxobutanato](2-)-N,N′,O3,O3′}, L2 = (3,3′)-[{1,2-phenylenebis(iminomethylidyne)]bis(2,4-pentane-dionato)(2-)-N,N′,O2,O2′}) and L3 being a octadentate dinucleating coordinating Schiff base like ligand ({tetraethyl-(E,E,E,E)-2,2′,2′′,2′′′-[1,2,4,5-phenylentetra(iminomethylidine)]tetra[3-oxobutanoato](2-)-N,N′,N′′,N′′′,O3,O3′,O3′′,O3′′′}); 4-dpa = di(4-picolyl)-amine, bipy = 4,4′-bipyridine, bpee = trans-1,2-bis(4-pyridyl)ethylene, 1-meim = 1-methylimidazole and DMAP = 4-dimethylaminopyridine, have been synthesized and characterised using X-ray structure analysis and T-dependent susceptibility measurements. Both methods indicate that all iron(II) centres are in the paramagnetic high-spin state over the whole temperature range investigated. The O-Fe-O angle, the so called bit of the equatorial ligand, is with an average of 111° in the region typical for high-spin iron(II) complexes of this ligand type. In the case of compound 1 an infinite two-dimensional hydrogen bond network can be found, for the compounds 2-4 no hydrogen bond interactions are observed between the complex molecules. A comparison of the curve progression obtained from the magnetic measurements of the mononuclear complex 5 and the polymeric complexes 1-3 leads to the conclusion that no magnetic interactions are mediated over the bridging axial ligands. For the dinuclear complex 4 weak antiferromagnetic interactions between the two iron centres are found.  相似文献   

20.
Bi-nuclear neutral sulfur-nitrosyl iron complex [Fe2(SR)2(NO)4] (I) has been obtained by replacement of thiosulfate ligands in dianion [Fe2(S2O3)2(NO)4]2− by 1-methyl-imidazole-2-yl. From X-ray analysis data, the complex has centrosymmetrical dimeric structure, with the iron atoms being linked via μ-N-C-S bridge. From Mossbauer spectroscopy, isomeric shift δFe is 0.180(1) mm/s and quadrupole splitting ΔEQ is 0.928(2) mm/s at T = 290 K. By comparative studying the mass-spectra in the gaseous phase of solid samples decomposition and kinetics of NO release in 1% aqueous solutions of dimethylsulfoxide, using of the ligand with CH3 substituent in position 1 of imidazole-2-thiol was shown to yield a more stable donor of nitrogen monoxide than earlier obtained analog with imidazole-2-thiol, [Fe2(C3H3N2S)2(NO)4].  相似文献   

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