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1.
The core–shell structure Fe3O4/SiO2 magnetic microspheres were prepared by a sol–gel method, and immobiled with iminodiacetic acid (IDA) as metal ion affinity ligands for protein adsorption. The size, morphology, magnetic properties and surface modification of magnetic silica nanospheres were characterized by various modern analytical instruments. It was shown that the magnetic silica nanospheres exhibited superparamagnetism with saturation magnetization values of up to 58.1 emu/g. Three divalent metal ions, Cu2+, Ni2+ and Zn2+, were chelated on the Fe3O4@SiO2–IDA magnetic microspheres to adsorb lysozyme. The results indicated that Ni2+‐chelating magnetic microspheres had the maximum adsorption capacity for lysozyme of 51.0 mg/g, adsorption equilibrium could be achieved within 60 min and the adsorbed protein could be easily eluted. Furthermore, the synthesized Fe3O4@SiO2–IDA–Ni2+ magnetic microspheres were successfully applied for selective enrichment lysozyme from egg white and His‐tag recombinant Homer 1a from the inclusion extraction expressed in Escherichia coli. The result indicated that the magnetic microspheres showed unique characteristics of high selective separation behavior of protein mixture, low nonspecific adsorption, and easy handling. This demonstrates that the magnetic silica microspheres can be used efficiently in protein separation or purification and show great potential in the pretreatment of the biological sample. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

2.
In this study, Ag, Ni2+, and Fe2+ immobilized on hydroxyapatite‐core‐shell γ‐Fe2O3 nanoparticles (γ‐Fe2O3@HAp‐Ag, γ‐Fe2O3@HAp‐Ni2+, and γ‐Fe2O3@HAp‐Fe2+) as a new and reusable Lewis acid magnetic nanocatalyst was successfully synthesized and reported for an atom economic, extremely facile, and environmentally benign procedure for the synthesis of highly functionalized tetrahydropyridines derivatives 4a‐t is described by one‐pot five‐component reaction of 2 equiv of aldehydes 1 , 2 equiv of amines 2 , and 1 equiv of methyl acetoacetate 3 in EtOH at room temperature in good to high yields and short reaction time. The presented methodology offers several advantages such as easy work‐up procedure, reusability of the magnetic nanocatalyst, operational simplicity, green synthesis avoiding toxic reagents and solvent, mild reaction conditions, and no tedious column chromatographic separation.  相似文献   

3.
This study describes the synthesis and characterization of ethylenediaminetetraacetic acid (EDTA) functionalized magnetic nanoparticles of 20 nm in size – Fe3O4@SiO2‐EDTA – which were used as a novel magnetic adsorbent for Cd(II) and Pb(II) binding in aqueous medium. These nanoparticles were obtained in two‐stage synthesis: covering by tetraethyl orthosilicate and functionalization with EDTA derivatives. Nanoparticles were characterized using TEM, FT‐IR, and XPS methods. Metal ions were detected under optimized experimental conditions using Differential Pulse Anodic Stripping Voltammetry (DPASV) and Hanging Mercury Drop Electrode (HDME) techniques. We compared the ability of Fe3O4@SiO2‐EDTA to bind cadmium and lead in concentration of 553.9 μg L?1 and 647.5 μg L?1, respectively. Obtained results show that the adsorption rate of cadmium binding was very high. The equilibrium for Fe3O4@SiO2‐EDTA‐Cd(II) was reached within 19 min while for the Fe3O4@SiO2‐EDTA‐Pb(II) was reached within 25 minutes. About 2 mg of nanoparticles was enough to bind 87.5 % Cd(II) and 54.1 % Pb(II) content. In the next step the binding capacity of Fe3O4@SiO2‐EDTA nanoparticles was determined. Only 1.265 mg of Fe3O4@SiO2‐EDTA was enough to bind 96.14 % cadmium ions while 5.080 mg of nanoparticles bound 40.83 % lead ions. This phenomenon proves that the studied nanoparticles bind Cd(II) much better than Pb(II). The cadmium ions binding capacity of Fe3O4@SiO2‐EDTA nanoparticles decreased during storage in 0.5 M KCl solution. Two days of Fe3O4@SiO2‐EDTA storage in KCl solution caused the 32 % increase in the amount of nanoparticles required to bind 60 % of cadmium while eight‐days storage caused further increase to 328 %. The performed experiment confirmed that the storage of nanoparticles in solution without any surfactants reduced their binding capacity. The best binding capacity was observed for the nanoparticles prepared directly before the electrochemical measurements.  相似文献   

4.
A type of fluorescent–magnetic dual‐function nanocomposite, Fe3O4@SiO2@P‐2, was successfully obtained by Cu+‐catalyzed click reaction between acetylene (C?C? H)‐substituted carbazole‐based conjugated polymer ( P‐2) and azide‐terminated silica‐coated magnetic iron oxide nanoparticles (Fe3O4@SiO2–N3). Optical and magnetization analyses indicate that Fe3O4@SiO2@P‐2 exhibits stable fluorescence and rapid magnetic response. The fluorescence of Fe3O4@SiO2@P‐2 was quenched significantly in the presence of I? and gave a detection limit (DL) of ~8.85 × 10?7 M. Given the high binding constant and matching ratio between Hg2+ and I?, the fluorescence of Fe3O4@SiO2@P‐2/I? complex recovered efficiently with the addition of Hg2+. A DL of ~4.17 × 10?7 M was obtained by this probing system. Recycling of Fe3O4@SiO2@P‐2 probe was readily achieved by simple magnetic separation. Results indicate that Fe3O4@SiO2@P‐2 can be used as an “on–off–on” fluorescent switchable and recyclable Hg2+ probe. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2013, 51, 3636–3645  相似文献   

5.
Ni2+‐complexed poly(2‐acetamidoacrylic acid) (PAAA) hydrogel beads were developed for the site‐specific reversible immobilization and purification of the histidine‐tagged green fluorescent protein (His‐tagged GFP). PAAA hydrogel beads were prepared by photopolymerization, and significantly improved mechanical properties of PAAA hydrogel beads were observed in comparison with PAAA hydrogel from our previous study. Confocal laser scanning microscopy was used to determine the binding of His‐tagged GFP to the hydrogel beads in three‐dimensional space. Photoluminescence spectroscopy revealed 89% of binding efficiency of His‐tagged GFP to the Ni2+‐PAAA hydrogel beads, 51% of yielding recovery. The maximum binding capacity of His‐tagged GFP was estimated to be 0.45 µg/mg of Ni2+‐PAAA hydrogel beads. The recombinant His‐tagged GFP from the soluble fraction of E. coli BL21(DE3) cell lysates was purified with Ni2+‐PAAA hydrogel beads. The major advantage of the Ni2+‐PAAA hydrogel beads system was simple preparation procedures of producing the matrix, because PAAA hydrogel beads had relatively enhanced mechanical strength than soft hydrogels. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

6.
An amino‐functionalized silica‐coated Fe3O4 nanocomposite (Fe3O4@SiO2/APTS) was synthesized. The Fe3O4@SiO2 microspheres possessed a well‐defined core–shell structure, uniform sizes and high magnetization. An immobilized ruthenium nanoparticle catalyst (Fe3O4@SiO2/APTS/Ru) was obtained after coordination and reduction of Ru3+ on the Fe3O4@SiO2/APTS nanocomposite. The Ru nanoparticles were not only ultra‐small with nearly monodisperse sizes but also had strong affinity with the surface of Fe3O4@SiO2/APTS. The obtained catalyst exhibited excellent catalytic performance for the hydrogenation of a variety of aromatic nitro compounds, even at room temperature. Moreover, Fe3O4@SiO2/APTS/Ru was easily recovered using a magnetic field and directly reused for at least five cycles without significant loss of its activity.  相似文献   

7.
Fe3O4@SiO2 nanoparticles was functionalized with a binuclear Schiff base Cu(II)‐complex (Fe3O4@SiO2/Schiff base‐Cu(II) NPs) and used as an effective magnetic hetereogeneous nanocatalyst for the N‐arylation of α‐amino acids and nitrogen‐containig heterocycles. The catalyst, Fe3O4@SiO2/Schiff base‐Cu(II) NPs, was characterized by Fourier transform infrared (FTIR) and ultraviolet‐visible (UV‐vis) analyses step by step. Size, morphology, and size distribution of the nanocatalyst were studied by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and dynamic light scatterings (DLS) analyses, respectively. The structure of Fe3O4 nanoparticles was checked by X‐ray diffraction (XRD) technique. Furthermore, the magnetic properties of the nanocatalyst were investigated by vibrating sample magnetometer (VSM) analysis. Loading content as well as leaching amounts of copper supported by the catalyst was measured by inductive coupled plasma (ICP) analysis. Also, thermal studies of the nanocatalyst was studied by thermal gravimetric analysis (TGA) instrument. X‐ray photoelectron spectroscopy (XPS) analysis of the catalyst revealed that the copper sites are in +2 oxidation state. The Fe3O4@SiO2/Schiff base‐Cu(II) complex was found to be an effective catalyst for C–N cross‐coupling reactions, which high to excellent yields were achieved for α‐amino acids as well as N‐hetereocyclic compounds. Easy recoverability of the catalyst by an external magnet, reusability up to eight runs without significant loss of activity, and its well stability during the reaction are among the other highlights of this catalyst.  相似文献   

8.
Novel Pd nanoparticles were prepared in five successive stages: 1) preparation of the Fe3O4 magnetic nanoparticles (Fe3O4 MNPs), 2) coating of Fe3O4 MNPs with SiO2 (Fe3O4@SiO2), 3) functionalization of Fe3O4@SiO2 with 3‐chloropropyltrimethoxy‐ silane (CPTMS) ligand (Fe3O4@SiO2@CPTMS), 4) further functionalization with 3,5‐diamino‐1,2,4‐triazole (DAT) ligand (Fe3O4@SiO2@CPTMS @DAT), and 5) the complexation of Fe3O4@SiO2@CPTMS@DAT with PdCl2 (Fe3O4@SiO2@CPTMS@ DAT@Pd). Then, the obtained Pd nano‐catalyst characterized by different methods such as the elemental analysis (CHN), FT‐IR, XRD, EDX, SEM, TEM, TG‐DTA and VSM. Finally, the Pd catalyst was applied for the synthesis of various 2‐imino‐3‐phenyl‐2,3‐dihydrobenzo[d]oxazol‐5‐ols.  相似文献   

9.
The catalytic activity of UiO‐66@Fe3O4@SiO2 catalyst was investigated in the fixation of carbon dioxide with epoxides under mild conditions. In this manner, a facile magnetization of UiO‐66 was achieved simultaneously by simply mixing this metal–organic framework and silica‐coated Fe3O4 nanoparticles in solution under sonication. The prepared catalyst was characterized using Fourier transform infrared and UV–visible spectroscopies, X‐ray diffraction, transmission and field emission scanning electron microscopies, N2 adsorption and inductively coupled plasma atomic emission spectroscopy. This new heterogeneous catalyst was applied as a highly efficient catalyst in the coupling of carbon dioxide with epoxides at mild temperatures and pressures. Furthermore, it could be easily recovered with the assistance of an external magnetic field and reused three consecutive times without significant loss of activity and mass.  相似文献   

10.
An advanced novel magnetic ionic liquid based on imidazolium tagged with ferrocene, a supported ionic liquid, is introduced as a recyclable heterogeneous catalyst. Catalytic activity of the novel nanocatalyst was investigated in one‐pot three‐component reactions of various aldehydes, malononitrile and 2‐naphthol for the facile synthesis of 2‐amino‐3‐cyano‐4H‐pyran derivatives under solvent‐free conditions without additional co‐catalyst or additive in air. For this purpose, we firstly synthesized and investigated 1‐(4‐ferrocenylbutyl)‐3‐methylimidazolium acetate, [FcBuMeIm][OAc], as a novel basic ferrocene‐tagged ionic liquid. This ferrocene‐tagged ionic liquid was then linked to silica‐coated nano‐Fe3O4 to afford a novel heterogeneous magnetic nanocatalyst, namely [Fe3O4@SiO2@Im‐Fc][OAc]. The synthesized novel catalyst was characterized using 1H NMR, 13C NMR, Fourier transform infrared and energy‐dispersive X‐ray spectroscopies, X‐ray diffraction, and transmission and field emission scanning electron microscopies. Combination of some unique characteristics of ferrocene and the supported ionic liquid developed the catalytic activity in a simple, efficient, green and eco‐friendly protocol. The catalyst could be reused several times without loss of activity.  相似文献   

11.
Functional polymer‐grafting silica nanoparticles hold great promise in diverse applications such as molecule recognition, drug delivery, and heterogeneous catalysis due to high density and uniform distribution of functional groups and their tunable spatial distance. However, conventional grafting methods from monomers mainly consist of one or more extra surface modification steps and a subsequent surface polymerization step. A monomer protonation‐dependent surface polymerization strategy is proposed to achieve one‐step uniform surface grafting of cross‐linked poly(4‐vinylpyridine) (P4VP) onto core–shell Fe3O4@SiO2 nanostructures. At an approximate pH, partially protonated 4VP sites in aqueous solution can be strongly adsorbed onto deprotonated silanol groups ( Si O) onto Fe3O4@SiO2 nanospheres to ensure prior polymerization of these protonated 4VP sites exclusively onto Fe3O4@SiO2 nanoparticles and subsequent polymerization of other 4VP and divinylbenzene monomers harvested by these protonated 4VP monomers onto Fe3O4@SiO2 nanoparticles, thereby achieving direct grafting of cross‐linked P4VP macromolecules onto Fe3O4@SiO2 nanoparticles.  相似文献   

12.
Magnetic particles with suitable surface modification are capable of binding proteins selectively, and magnetic separations have advantages of rapidity, convenience, and high selectivity. In this paper, new magnetic nanoparticles modified with imidazolium ionic liquid (Fe3O4@SiO2@ILs) were successfully fabricated. N‐Methylimidazolium was immobilized onto silica‐coated magnetic nanoparticles via γ‐chloropropyl modification as a magnetic nanoadsorbent for heme protein separation. The particle size was about 90 nm without significant aggregation during the preparation process. Hemoglobin as one of heme proteins used in this experiment was compared with other nonheme proteins. It has been found that the magnetic nanoparticles can be used for more rapid, efficient, and specific adsorption of hemoglobin with a binding capacity as high as 5.78 mg/mg. In comparison with other adsorption materials of proteins in the previous reports, Fe3O4@SiO2@ILs magnetic nanoparticles exhibit the excellent performance in isolation of heme proteins with higher binding capacity and selectivity. In addition, a short separation time makes the functionalized nanoparticles suitable for purifying unstable proteins, as well as having other potential applications in a variety of biomedical fields.  相似文献   

13.
A typical superparamagnetic nanoparticles-based dithiocarbamate absorbent (Fe3O4@SiO2-DTC) with core-shell structure was applied for aqueous solution heavy metal ions Ni2+, Cu2+ removal.  相似文献   

14.
We adopted a facile hydrofluoric acid‐free hydro‐/solvothermal method for the preparation of four magnetic iron(III)‐based framework composites (MIL‐101@Fe3O4‐COOH, MIL‐101‐NH2@Fe3O4‐COOH, MIL‐53@Fe3O4‐COOH, and MIL‐53‐NH2@Fe3O4‐COOH). The obtained four magnetic iron(III)‐based framework composites were applied to magnetic separation and enrichment of the fungicides (prochloraz, myclobutanil, tebuconazole, and iprodione) from environmental samples before high‐performance liquid chromatographic analysis. MIL‐101‐NH2@Fe3O4‐COOH showed more remarkable pre‐concentration ability for the fungicides as compared to the other three magnetic iron(III)‐based framework composites. The extraction parameters affecting enrichment efficiency including extraction time, sample pH, elution time, and the desorption solvent were investigated and optimized. Under the optimized conditions, the standard curve of correlation coefficients were all above 0.991, the limits of detection were 0.04–0.4 μg/L, and the relative standard deviations were below 10.2%. The recoveries of two real water samples ranged from 71.1–99.1% at the low spiking level (30 μg/L). Therefore, the MIL‐101‐NH2@Fe3O4‐COOH composites are attractive for the rapid and efficient extraction of fungicides from environmental water samples.  相似文献   

15.
A biosensor based on hemoglobin‐Fe3O4@SiO2 nanoparticle bioconjunctions modified indium‐tin‐oxide (Hb/Fe3O4@SiO2/ITO) electrode was fabricated to determine the concentration of H2O2. UV‐vis absorption spectra, fourier transform infrared (FT‐IR) spectroscopy, cyclic voltammetry (CV) and high‐resolution transmission electron microscopy (HRTEM) were used to characterize the bioconjunction of Fe3O4@SiO2 with Hb. Experimental results demonstrate that the immobilized Hb on the Fe3O4@SiO2 matrix retained its native structure well. In addition, Fe3O4@SiO2 nanoparticles (NPs) are very effective in facilitating electron transfer of the immobilized enzyme, which can be attributed to the unique nanostructure and larger surface area of the Fe3O4@SiO2 NPs. The biosensor displayed good performance for the detection of H2O2 with a wide linear range from 2.03×10?6 to 4.05×10?3 mol/L and a detection limit of 0.32 µmol/L. The resulting biosensor exhibited fast amperometric response, good stability, reproducibility, and selectivity to H2O2.  相似文献   

16.
The surface of Fe3O4@SiO2 nanoparticles was modified using l ‐arginine as a green and available amino acid to trap palladium nanoparticles through a strong interaction between the metal nanoparticles and functional groups of the amino acid. The proposed green synthetic method takes advantage of nontoxic reagents through a simple procedure. Characterization of Fe3O4@SiO2@l ‐arginine@Pd(0) was done using Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, X‐ray diffraction, vibrating sample magnetometry and inductively coupled plasma analysis. The catalytic activity of Fe3O4@SiO2@l ‐arginine@Pd(0) as a new nanocatalyst was investigated in C – C coupling reactions. Waste‐free, use of green medium, efficient synthesis leading to high yield of products, eco‐friendly and economic catalyst, excellent reusability of the nanocatalyst and short reaction time are the main advantages of the method presented. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

17.
A highly porous metal‐organic framework, MIL‐101(Fe), was prepared by a solvothermal method in the presence of amino‐modified Fe3O4@SiO2 nanoparticles, in order to achieve Fe3O4/MIL‐101(Fe) nanocomposite, which was characterized by XRD, FT‐IR, SEM, TEM, BET, and VSM. This hybrid magnetic nanocomposite was employed as heterogeneous catalyst for α‐amino nitriles synthesis through three‐component condensation reaction of aldehydes (ketones), amines, and trimethylsilyl cyanide in EtOH, at room temperature. The recoverability and reusability was admitted for the heterogeneous magnetic catalyst; no significant reduction of catalytic activity was observed even after five consecutive reaction cycles.  相似文献   

18.
New functionalized magnetic core–shell nanoparticles, CuFe2O4@SiO2‐OP2O5H, were prepared by grafting of phosphorus pentoxide on CuFe2O4@SiO2 nanoparticles and characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, energy‐dispersive X‐ray analysis, inductively coupled plasma optical emission spectrometry and vibrating sample magnetometry. The catalytic activity of CuFe2O4@SiO2‐OP2O5H as a novel catalyst was evaluated in the synthesis of 1,8‐dioxo‐octahydroxanthenes under solvent‐free conditions. The results showed that the catalyst has high activity and the desired products are obtained in high yields within short reaction times. The catalyst is readily recovered using magnetic decantation and can be used at least four times without noticeable deterioration in catalytic activity.  相似文献   

19.
CoFe2O4@SiO2‐CPTES‐Guanidine‐Cu(II) magnetic nanoparticles were synthesized and used as a new, inexpensive and efficient heterogeneous catalyst for the synthesis of polyhydroquinolines and 2,3‐dihydroquinazoline‐4(1H)‐ones and for the oxidation of sulfides. The structure of this nanocatalyst was characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, vibrating sample magnetometry, thermogravimetric analysis, X‐ray diffraction and inductively coupled plasma optical emission spectrometry. Simple preparation, high catalytic activity, simple operation, high yields, use of green solvents, easy magnetic separation and reusability of the catalyst are some of the advantages of this protocol.  相似文献   

20.
Butane‐1‐sulfonic acid immobilized on magnetic Fe3O4@SiO2 nanoparticles (Fe3O4@SiO2‐Sultone) was easily prepared via direct ring opening of 1,4‐butanesultone with nanomagnetic Fe3O4@SiO2. The prepared reagent was characterized and used for the efficient promotion of the synthesis of barbituric acid and pyrano[2,3‐d] pyrimidine derivatives. All reactions were performed under mild and completely heterogeneous reaction conditions affording products in good to high yields. The catalyst is easily isolated from the reaction mixture by magnetic decantation and can be reused at least eight times without significant loss in activity.  相似文献   

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