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1.
Magnetic silica‐coated magnetite (Fe3O4) sub‐microspheres with immobilized metal‐affinity ligands are prepared for protein adsorption. First, magnetite sub‐microspheres were synthesized by a hydrothermal method. Then silica was coated on the surface of Fe3O4 particles using a sol–gel method to obtain magnetic silica sub‐microspheres with core‐shell morphology. Next, the trichloro(4‐chloromethylphenyl) silane was immobilized on them, reacted with iminodiacetic acid (IDA), and charged with Cu2+. The obtained magnetic silica sub‐microspheres with immobilized Cu2+ were applied for the absorption of bovine hemoglobin (BHb) and the removal of BHb from bovine blood. The size, morphology, and magnetic properties of the resulting magnetic micro(nano) spheres were investigated by using scanning microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), and a vibrating sample magnetometer (VSM). The measurements showed that the magnetic sub‐microspheres are spherical in shape, very uniform in size with a core‐shell, and are almost superparamagnetic. The saturation magnetization of silica‐coated magnetite (Fe3O4) sub‐microspheres reached about 33 emu g?1. Protein adsorption results showed that the sub‐microspheres had a high adsorption capacity for BHb (418.6 mg g?1), low nonspecific adsorption, and good removal of BHb from bovine blood. This opens a novel route for future applications in removing abundant proteins in proteomic analysis.  相似文献   

2.
Employing immobilized metal‐ion affinity chromatography and magnetic separation could ideally provide a useful analytical strategy for purifying His‐tagged protein. In the current study, a facile route was designed to prepare CMPEI‐Ni2+@SiO2@Fe3O4 (CMPEI=carboxymethylated polyethyleneimine) magnetic nanoparticles composed of a strong magnetic core of Fe3O4 and a Ni2+‐immobilized carboxymethylated polyethyleneimine coated outside shell, which was formed by electrostatic interactions between polyanionic electrolyte of carboxymethylated polyethyleneimine and positively charged surface of 3‐(trimethoxysilyl)propylamin modified SiO2@Fe3O4. The resulting CMPEI‐Ni2+@SiO2@Fe3O4 composite nanoparticles displayed well‐uniform structure and high magnetic responsiveness. Hexa His‐tagged peptides and purified His‐tagged recombinant retinoid X receptor alpha were chosen as the model samples to evaluate the adsorption, capacity, and reusability of the composite nanoparticles. The results demonstrated the CMPEI‐Ni2+@SiO2@Fe3O4 nanoparticles possessed rapid adsorption, large capacity, and good recyclability. The obtained nanoparticles were further used to purify His‐tagged protein in practical environment. It was found that the nanoparticles could selectively capture His‐tagged recombinant retinoid X receptor protein from complex cell lysate. Owing to its easy synthesis, large binding capacity, and good reusability, the prepared CMPEI‐Ni2+@SiO2@Fe3O4 magnetic nanoparticles have great potential for application in biotechnological fields.  相似文献   

3.
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   

4.
Silica (SiO2) nanospheres (NSs) with immobilized metal ligands have been prepared for the affinity separation of proteins. First, SiO2 NSs were prepared by controlled hydrolysis of tetraethoxysilane in a basic aqueous-ethanol solution. Then through reaction of iminodiacetic acid (IDA) with 3-glycidoxypropyltrimethoxysilane and immobilization of them onto the surfaces of above SiO2 NSs, novel affinity adsorbents with IDA chelating groups were obtained. After chelating Ni2+ ions, the SiO2–IDA–Ni2+ NSs were applied to separate his-tagged proteins directly from the mixture of lysed cells. The SiO2–IDA–Ni2+ NSs present negligible nonspecific protein adsorption and high protein binding ability (28.3 mg/g).  相似文献   

5.
采用“一锅法”制备了四氧化三铁/半胱氨酸(Fe3O4/Cys)磁性纳米微球,随后对Fe3O4/Cys进行亚氨基二乙酸(IDA)修饰得到Fe3O4/Cys/IDA磁性双功能化纳米微球。研究发现Fe3O4/Cys中的L-Cys是通过—SH基团接枝到Fe3O4表面的,随后IDA分子中的羧基与Fe3O4/Cys中的—NH2形成酰胺键,最终形成多支链多羧基的Fe3O4/Cys/IDA磁性纳米修复剂。基于修复剂表面短支链-长支链交替的多羧基结构,实现了羧基基团的高密度接枝。同时,Fe3O4/Cys/IDA磁性纳米微球对Pb2+、Cd2+、Cu2+、Co2+、Ni2+、Zn2+为专性吸附,而对Hg2+属于非专性吸附,且吸附重金属后得到的钝化产物均表现了良好的稳定性。另外,Fe3O4/Cys/IDA对重金属离子的吸附符合Langmuir模型,属于单层均相吸附,其吸附过程符合准二级动力学模型,最大吸附量为49.05 mg·g-1。  相似文献   

6.
Monodisperse metal clusters provide a unique platform for investigating magnetic exchange within molecular magnets. Herein, the core–shell structure of the monodisperse molecule magnet of [Gd52Ni56(IDA)48(OH)154(H2O)38]@SiO2 ( 1 a @SiO2) was prepared by encapsulating one high‐nuclearity lanthanide–transition‐metal compound of [Gd52Ni56(IDA)48(OH)154(H2O)38]?(NO3)18?164 H2O ( 1 ) (IDA=iminodiacetate) into one silica nanosphere through a facile one‐pot microemulsion method. 1 a @SiO2 was characterized using transmission electron microscopy, N2 adsorption–desorption isotherms, and inductively coupled plasma‐atomic emission spectrometry. Magnetic investigation of 1 and 1 a revealed J1=0.25 cm?1, J2=?0.060 cm?1, J3=?0.22 cm?1, J4=?8.63 cm?1, g=1.95, and z J=?2.0×10?3 cm?1 for 1 , and J1=0.26 cm?1, J2=?0.065 cm?1, J3=?0.23 cm?1, J4=?8.40 cm?1 g=1.99, and z J=0.000 cm?1 for 1 a @SiO2. The z J=0 in 1 a @SiO2 suggests that weak antiferromagnetic coupling between the compounds is shielded by silica nanospheres.  相似文献   

7.
An effective one‐pot, convenient process for the synthesis of 1‐ and 5‐substituted 1H‐tetrazoles from nitriles and amines is described using1,4‐dihydroxyanthraquinone–copper(II) supported on Fe3O4@SiO2 magnetic porous nanospheres as a novel recyclable catalyst. The application of this catalyst allows the synthesis of a variety of tetrazoles in good to excellent yields. The preparation of the magnetic nanocatalyst with core–shell structure is presented by using nano‐Fe3O4 as the core, tetraethoxysilane as the silica source and poly(vinyl alcohol) as the surfactant, and then Fe3O4@SiO2 was coated with 1,4‐dihydroxyanthraquinone–copper(II) nanoparticles. The new catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, thermogravimetric analysis, vibration sample magnetometry, X‐ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm analysis and inductively coupled plasma analysis. This new procedure offers several advantages such as short reaction times, excellent yields, operational simplicity, practicability and applicability to various substrates and absence of any tedious workup or purification. In addition, the excellent catalytic performance, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. Also, the catalyst could be magnetically separated and reused six times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

8.
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   

9.
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   

10.
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   

11.
The effect of radioactive UO22+ on the oxygen‐transporting capability of hemoglobin‐based oxygen carriers has been investigated in vitro. The hemoglobin (Hb) microspheres fabricated by the porous template covalent layer‐by‐layer (LbL) assembly were utilized as artificial oxygen carriers and blood substitutes. Magnetic nanoparticles of iron oxide (Fe3O4) were loaded in porous CaCO3 particles for magnetically assisted chemical separation (MACS). Through the adsorption spectrum of magnetic Hb microspheres after adsorbing UO22+, it was found that UO22+ was highly loaded in the magnetic Hb microspheres, and it shows that the presence of UO22+ in vivo destroys the structure and oxygen‐transporting capability of Hb microspheres. In view of the high adsorption capacity of UO22+, the as‐assembled magnetic Hb microspheres can be considered as a novel, highly effective adsorbent for removing metal toxins from radiation‐contaminated bodies, or from nuclear‐power reactor effluent before discharge into the environment.  相似文献   

12.
A protein imprinting approach for the synthesis of core–shell structure nanoparticles with a magnetic core and molecularly imprinted polymer (MIP) shell was developed using a simple distillation–precipitation polymerization method. In this work, Fe3O4 magnetic nanoparticles were first synthesized through a solvothermal method and then were conveniently surface‐modified with 3‐(methacryloyloxy)propyltrimethoxylsilane as anchor molecules to donate vinyl groups. Next a high‐density MIP shell was coated onto the surface of the magnetic nanoparticles by the copolymerization of functional monomer acrylamide (AAm), cross‐linking agent N,N′‐methylenebisacrylamide (MBA), the initiator azodiisobutyronitrile (AIBN), and protein in acetonitrile heated at reflux. The morphology, adsorption, and recognition properties of the magnetic molecularly imprinted nanoparticles were investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), and rebinding experiments. The resulting MIP showed a high adsorption capacity (104.8 mg g?1) and specific recognition (imprinting factor=7.6) to lysozyme (Lyz). The as‐prepared Fe3O4@Lyz‐MIP nanoparticles with a mean diameter of 320 nm were coated with an MIP shell that was 20 nm thick, which enabled Fe3O4@Lyz‐MIP to easily reach adsorption equilibrium. The high magnetization saturation (40.35 emu g?1) endows the materials with the convenience of magnetic separation under an external magnetic field and allows them to be subsequently reused. Furthermore, Fe3O4@Lyz‐MIP could selectively extract a target protein from real egg‐white samples under an external magnetic field.  相似文献   

13.
Novel poly(deep eutectic solvent) grafted silica-coated magnetic microspheres (Fe3O4@SiO2-MPS@PDES) were prepared by polymerization of choline chloride-itaconic acid (ChCl-IA) and γ-MPS-modified magnetic silica composites, and were characterized by vibrating sample magnetometer (VSM), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectra (XPS), thermal gravimetric analysis (TGA) and transmission electron microscope (TEM). Then the synthetic Fe3O4@SiO2-MPS@PDES microspheres were applied for the magnetic solid-phase extraction (MSPE) of trypsin for the first time. After extraction, the concentration of trypsin in the supernatant was determined by a UV–vis spectrophotometer. Single factor experiments were carried out to investigate the effects of the extraction process, including the concentration of trypsin, the ionic strength, the pH value, the extraction time and the temperature. Experimental results showed the extraction capacity could reach up to 287.5 mg/g under optimized conditions. In comparison with Fe3O4@SiO2-MPS, Fe3O4@SiO2-MPS@PDES displayed higher extraction capacity and selectivity for trypsin. According to the regeneration studies, Fe3O4@SiO2-MPS@PDES microspheres can be recycled six times without significant loss of its extraction capacity, and retained a high extraction capacity of 233 mg/g after eight cycles. Besides, the activity studies also demonstrated that the activity of the extracted trypsin was well retained. Furthermore, the analysis of real sample revealed that the prepared magnetic microspheres can be used to purify trypsin in crude bovine pancreas extract. These results highlight the potential of the proposed Fe3O4@SiO2-MPS@PDES-MSPE method in separation of biomolecules.  相似文献   

14.
In this paper, magnetic chitosan microspheres were prepared by the emulsification cross-linking technique, with glutaraldehyde as the cross-linking agent, liquid paraffin as the dispersant, and the Span-80 as emulsifier. The time of cross-linking and the ratio of Co0.5Ni0.5Fe2O4/chitosan were investigated. The morphology was studied by different instruments. The adsorption performance was investigated and the effects of initial concentration of methyl orange, the time of cross-linking, and the amount of adsorbent were discussed. It is found that the product has uniform morphology when the ratio of magnetic Co0.5Ni0.5Fe2O4/chitosan is 1 : 2 and the time of cross-linking is 5 h; At room temperature, magnetic Co0.5Ni0.5Fe2O4–chitosan has a good adsorption toward methyl orange when the magnetic Co0.5Ni0.5Fe2O4/chitosan dosage is 20 mg.  相似文献   

15.
ABSTRACT

In this work, a magnetic molecularly imprinted polymer (Fe3O4@SiO2@MIPs) was prepared via a surface-imprinted method for the determination of the triazines in environmental water samples combined with high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). The Fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer showed that the Fe3O4@SiO2@MIPs was successfully synthesised and exhibited superparamagnetism. The isotherm adsorption, selectivity and adsorption kinetics experiments showed that the Fe3O4@SiO2@MIPs exhibited excellent specific recognition and fast adsorption equilibrium for triazines. The adsorption process is spontaneous and endothermic. The isotherm adsorption was consistent with Scatchard model and adsorption kinetic fit pseudo-second-order kinetic model. Under the optimised adsorption conditions, the Fe3O4@SiO2@MIPs was directly used to selectively enrich six triazines in environmental water samples. The enrichment volume was up to 500 mL, and the matrix effects were down to 0.7–12.4%. The built method has excellent linearities in the range of 0.25–500 ng L?1 with R2 in the range of 0.998–0.999, lower limit of detections (0.02–0.08 ng L?1) and higher precision (2.4–7.2%). The Fe3O4@SiO2@MIPs is expected to be widely applied to the direct enrichment of triazines in bulk environmental water samples.  相似文献   

16.
In this study, the synthesis of sulfonic acid supported on ferrite–silica superparamagnetic nanoparticles (Fe3O4@SiO2@SO3H) as a nanocatalyst with large density of acidic groups is suggested. This nanocatalyst was prepared in three steps: preparation of colloidal iron oxide magnetic nanoparticles (Fe3O4 MNPs), coating of silica on Fe3O4 MNPs (Fe3O4@SiO2) and incorporation of sulfonic acid as a functional group on the surface of Fe3O4@SiO2 nanoparticles (Fe3O4@SiO2@SO3H). The properties of the prepared magnetic nanoparticles were characterized using transmission electron microscopy, infrared spectroscopy, vibrating sample magnetometry, X‐ray diffraction and thermogravimetric analysis. Finally, the applicability of the synthesized magnetic nanoparticles was tested as a heterogeneous solid acid nanocatalyst for one‐pot synthesis of diindolyloxindole derivatives in aqueous medium. Oxindole derivatives were produced by the coupling of indole and isatin compounds with good to high yields (60–98%). Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

17.
The adsorption of the dyes Acid Red 114 and Reactive Black 5 in aqueous solutions on polyhydroxyl dendrimer magnetic nanoparticles (Fe3O4@SiO2‐TRIS) was studied in a batch system. The Fe3O4@SiO2‐TRIS NPs were characterized by Fourier transform infrared spectroscopy, X‐ray diffraction, and transmission electron microscopy. Experiments were performed under different conditions such as the initial dye concentration, adsorbent dose, and pH. The pseudo‐second‐order model provided a very good fit for the two anionic dyes. The Langmuir and Freundlich adsorption models were used to describe the equilibrium isotherms at different temperatures, and the former agreed very well with the experimental data. However, the adsorption capacity of Fe3O4@SiO2‐TRIS NPs was reduced during surface modification, which could be due to the dye occupying the binding sites of the dendrimer. Thermodynamic parameters, namely the change in free energy (ΔG0), enthalpy (ΔH0), and entropy (ΔS0), were also determined.  相似文献   

18.
Nanostructured carbon-based materials, such as carbon nanotube arrays have shown respectable removal ability for heavy metal ions and organic dyes in aqueous solution. Although the carbon-based materials exhibited excellent removal ability, the separation of them from the aqueous solution is difficult and time-consuming. Here we demonstrated a novel and facile route for the large-scale fabrication of Fe3O4@C hollow nanospheres, with using ferrocene as a single reagent and SiO2 as a template. The as-prepared Fe3O4@C hollow nanospheres exhibited adsorption ability for heavy metal ions and organic dyes from aqueous solution, and can be easily separated by an external magnet. When the as-prepared Fe3O4@C hollow nanospheres were mixed with the aqueous solution of Hg2+ within 15 min, the removal efficiency was 90.3%. The as-prepared Fe3O4@C hollow nanospheres were also exhibited a high adsorption capacity (100%) as the adsorbent for methylene blue (MB). In addition, the as-prepared Fe3O4@C hollow nanospheres can be used as the recyclable sorbent for water treatment via a simple magnetic separation.  相似文献   

19.
Iron oxide (Fe3O4) magnetic nanoparticles as movable cores were used to synthesize yolk–shell nanoparticles with pH‐responsive shell composed of ethylene glycol dimethacrylate (EGDMA)‐crosslinked poly(acrylic acid) (PAA) via two different routes. In the first more common route, Fe3O4 nanoparticles were coated with silica layer via the Stöber process to yield Fe3O4@SiO2 core–shell nanoparticles, subsequently used as seeds in the distillation precipitation copolymerization of AA and EGDMA to yield Fe3O4@SiO2@P(AA‐EGDMA). The silica layer was selectively removed through alkali etching to yield Fe3O4@air@P(AA‐EGDMA). In the second route, Fe3O4 nanoparticles without any stabilization were used as seeds in the distillation precipitation copolymerization of AA and EGDMA to yield Fe3O4@P(AA‐EGDMA) core–shell nanoparticles. The nanoparticles were subsequently dispersed in acidic medium of pH = 2. Yolk–shell Fe3O4@air@P(AA‐EGDMA) nanoparticles were formed through deswelling of crosslinked PAA because of protonation of carboxyl groups at low pH values. Various techniques were utilized to investigate the characteristics of the synthesized core–shell nanoparticles. Formation of yolk–shell nanostructure was observed for both synthesis routes, namely etching of silica layer and deswelling approaches, from vibrating sample magnetometry and transmission electron microscopy results. Both types of nanoparticles showed pH‐responsive behaviour, i.e. decrease in absorption with increase in pH, as examined using UV–visible spectroscopy.  相似文献   

20.
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   

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