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
Three‐dimensional graphene‐supported mesoporous silica@Fe3O4 composites (mSiO2@Fe3O4‐G) were prepared by modifying mesoporous SiO2‐coated Fe3O4 onto hydrophobic graphene nanosheets through a simple adsorption co‐condensation method. The obtained composites possess unique properties of large surface area (332.9 m2/g), pore volume (0.68 cm3/g), highly open pore structure with uniform pore size (31.1 nm), as well as good magnetic separation properties. The adsorbent (mSiO2@Fe3O4‐G) was used for the magnetic solid‐phase extraction of seven pesticides with benzene rings in different aqueous samples before high‐performance liquid chromatography. The main parameters affecting the extraction such as adsorbent amount, volume of elution solvent, time of extraction and desorption, salt effect, oscillation rate were investigated. Under the optimal conditions, this method provided low limits of detection (S/N = 3, 0.525–3.30 μg/L) and good linearity (5.0–1000 μg/L, R2 > 0.9954). Method validation proved the feasibility of the developed adsorbent, which has a high extraction efficiency and excellent enhancement performance for pesticides in this study. The proposed method was successfully applied to real aqueous samples, and satisfactory recoveries ranging from 77.5 to 113.6% with relative standard deviations within 9.7% were obtained. 相似文献
An aptamer (Apt) functionalized magnetic material was prepared by covalently link Apt to Fe3O4/graphene oxide (Fe3O4/GO) composite by 1‐ethyl‐3‐(3‐dimethylaminopropyl) carbodiimide hydrochloride and N‐hydroxysuccinimide, and then characterized by FTIR spectroscopy, X‐ray diffraction, and vibration sample magnetometry. The obtained composite of Fe3O4/GO/Apt was employed as magnetic solid‐phase extraction adsorbent for the selective preconcentration of sulfadimethoxine prior to analysis by high‐performance liquid chromatography. Under the optimal conditions (sample pH of 4.0, sorbent dosage of 20 mg, extraction time of 3 h, and methanol‐5% acetic acid solution as eluent), a good linear relationship was obtained between the peak area and concentration of sulfadimethoxine in the range of 5.0 to 1500.0 µg/L with correlation coefficient of 0.9997. The limit of detection (S/N = 3) was 3.3 µg/L. The developed method was successfully applied to the analysis of sulfadimethoxine in milk with recoveries in the range of 75.9‐92.3% and relative standard deviations less than 8.1%. The adsorption mechanism of Fe3O4/GO/Apt toward sulfadimethoxine was studied through the adsorption kinetics and adsorption isotherms, and the results show that the adsorption process fits well with the pseudo‐second‐order kinetic model and the adsorbate on Fe3O4/GO/Apt is multilayer and heterogeneous. 相似文献
Fe3O4@MCM‐41@Zr‐MNPs modified with piperazine is easily prepared and characterized using Fourier transform infrared spectroscopy (FT‐IR), X‐ray powder diffraction (XRD), N2 adsorption–desorption, Transmission electron microscopy (TEM), Energy‐dispersive X‐ray (EDX), Vibrating sample magnetometry (VSM) and Thermogravimetric analysis (TGA) techniques. The characterization results showed that Zr highly dispersed in the tetrahedral environment of silica framework and piperazine is successfully attached to the surface of the nanocatalyst in connection with zirconium. The prepared nanosized reagent (10–30 nm), shows excellent catalytic activity in the synthesis of tetrahydro‐4H‐chromene and pyrano[2,3‐d]pyrimidinone derivatives. All reactions are performed under mild and completely heterogeneous reactions conditions in high yields during short reaction times. On the other hand and due to its superparamagnetic nature the catalyst can be easily separated by the application of an external magnetic field and reused for several times. 相似文献
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
A novel Prussian blue (PB)‐Fe3O4 composite has been prepared for the first time by self‐template method using PB as the precursor. According to this method, Fe3O4 nanoparticles distributed uniformly on the surface of PB cube. The feed ratio of sodium acetate to PB has been proved to be a key factor for magnetic properties and electro‐catalysis properties of the composite. Under the experimental conditions, the saturation magnetization value (Ms) of PB‐Fe3O4–2 composite was 22 emug?1, while the Ms value of other samples reduced. The composites also showed a good peroxidase‐like activity for the oxidation of substrate 3,3,5,5‐tetramethylbenzidine (TMB) in the presence of H2O2. The catalytic reduction of hydrogen peroxide capacity was PB‐Fe3O4–1> PB‐Fe3O4–2> PB‐Fe3O4–3> PB‐Fe3O4–0, which confirmed the Fe(II) centres in PB surface and Fe3O4 nanoparticles had synergistic effect on catalytic reduction of hydrogen peroxide. 相似文献
The 4-sulfonylcalix[6]arene modified Fe3O4 (MFS) was characterized by FT-IR, SEM, VSM, TGA, etc., which showed that its saturation magnetization was 64.99 emu g?1 with the particle size 10–40 nm. The maximum adsorption efficiency by MFS for 2.5 mg L?1 U(VI) solution amounted to 94.39%, which was higher than that by Fe3O4 (65.22%) under its optimum adsorption conditions. The adsorption of MFS and Fe3O4 were both followed the pseudo-second order model and the Langmuir isotherm model. The Gibbs free energy change and enthalpy change revealed that the adsorption of U(VI) by MFS was a spontaneous and endothermic process. 相似文献
In this work, we report the development of novel amino-functionalized Fe3O4 hybrid microspheres adsorbent from a facial and one-step solvothermal route by using FeCl3·6H2O as a single iron source and 3-aminophenoxy-phthalonitrile as ource of amino groups. During solvothermal process, the nitrile groups of 3-aminophenoxy-phthalonitrile would bond with the Fe3O4 through the phthalocyanine cyclization reaction to form the amino-functionalized Fe3O4 magnetic nano-material, which was confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermo-gravimetric analyzer (TGA). From the scanning electron microscope (SEM) and transmission electron microscopy (TEM) observation, the resulting monodispersed amino-functionalized Fe3O4 hybrid microspheres with the diameters of 180–200 nm were synthesized via the self-assembly process. More importantly, as-prepared Fe3O4 nano-materials with abundant amino groups exhibited high separation efficiency when they were used to remove the Cu(II) from aqueous solutions. Furthermore, the adsorption isotherms of Fe3O4 nano-material for Cu(II) removal fitted the Langmuir isotherm model, in which the calculated maximum adsorption capacity could increase from 5.51 to 16.25 mg g–1 at room temperature. This work demonstrated that the amino-functionalized Fe3O4 magnetic nano-materials were promising as efficient adsorbents for the removal of heavy metal ions from wastewater in low concentration. 相似文献
The catalytic activity of l ‐arginine‐coated nano‐Fe3O4 particles (Fe3O4@l ‐arginine) proves they are a novel magnetic catalyst without the use of heat and reflux for the synthesis of 1,3‐diaryl‐2‐N‐azaphenalene derivatives and n‐acyl‐1,3‐diaryl‐2‐N‐azaphenylene derivatives in a one‐pot pseudo‐five‐component condensation reaction of compounds of 2,7‐naphthalene diol, aldehydes, and ammonia derivatives (ammonium acetate or ammonium hydrogen phosphate) and solvent (water and alcohol) with high yield and short reaction times, economical, and simple workup. The structure and magnetic properties of the obtained nanoparticles were characterized via Fourier transform infrared spectroscopy (IR) and field emission scanning electron microscopy (FE‐SEM). The results demonstrated that the average size of the synthesized magnetite nanoparticles is about 21 nm. In addition, the heterogeneous catalyst can be easily recovered magnetically and can be reused for further runs without significant loss of its catalytic activity. 相似文献
The ever‐increasing resistance of plant microbes towards fungicides and bactericides has been causing serious threat to plant production in recent years. For the development of an effective antifungal agent, we introduce a novel hydrothermal protocol for synthesis of chitosan iron oxide nanoparticles (CH‐Fe2O3 NPs) using acetate buffer of low pH 5.0 for intermolecular interaction of Fe2O3 NPs and CH. The composite structure and elemental elucidation were carried out by using X‐ray power diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X‐ray (EDX), Transmission Electron Microscopy (TEM), Fourier Transformed Infrared Spectroscopy (FTIR) and Ultraviolet Visible Absorption Spectroscopy (UV–vis spectroscopy). Additionally, antifungal activity was evaluated both In vitro and In vivo against Rhizopus oryzae which is causing fruit rot disease of strawberry. We compared different concentrations (0.25%, 0.50%, 075% and 1%) of CH‐Fe2O3 NPs and 50% synthetic fungicide (Matalyxal Mancozab) to figure out suitable concentration for application in the field. XRD analysis showed a high crystalline nature of the NPs with average size of 52 nanometer (nm). SEM images revealed spherical shape with size range of 50–70 nm, whereas, TEM also revealed spherical shape, size ranging from 0 nm to 80 nm. EDX and FTIR results revealed presence of CH on surface of Fe2O3 NPs. The band gap measurement showed peak 317–318 nm for bare Fe2O3 NPs and CH‐Fe2O3 NPs respectively. Antifungal activity in both In vitro and In vivo significantly increased with increase in concentration. The overall results revealed high synergetic antifungal potential of organometallic CH‐Fe2O3 NPs against Rhizopus oryzae and suggest the use of CH‐Fe2O3 NPs against other Phyto‐pathological diseases due to biodegradable nature. 相似文献
The first synthesis of porous, optically active, magnetic Fe3O4@poly(N‐acryloyl‐leucine) inverse core/shell composite microspheres is reported, in which the core is constructed of chiral polymer and the shell is constructed of Fe3O4 NPs. The microspheres integrate three significant concepts, “porosity”, “chirality”, and “magneticity”, in one single microspheric entity. The microspheres consist of Fe3O4 nanoparticles and porous optically active microspheres, and thus combine the advantages of both magnetic nanoparticles and porous optically active microspheres. The pore size and specific surface area of the microspheres are characterized by N2 adsorption, from which it is found that the composite microspheres possess a desirable porous structure. Circular dichroism and UV‐vis absorption spectroscopy measurements demonstrate that the microspheres exhibit the expected optical activity. The microspheres also have high saturation magnetization of 14.7 emu g–1 and rapid magnetic responsivity. After further optimization, these novel microspheres may potentially find applications in areas such as asymmetric catalysis, chiral adsorption, etc.
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
A nanostructured iron oxide (NanoFe3O4, particle size ca. 25 nm and roughness ca. 21 nm) film deposited onto a hydrolyzed indium‐tin‐oxide (ITO) coated glass plate has been used to immobilize cholesterol oxidase (ChOx) to fabricate an impedimetric cholesterol sensor. Electrochemical studies reveal that surface charged Fe3O4 nanoparticles provide better conformation for ChOx loading resulting in enhanced electron transfer between ChOx and the electrode. Impedimetric response studies of the ChOx/NanoFe3O4/ITO bioelectrode exhibit improved linearity (2.5–400 mg/dL), low detection limit (0.25 mg/dL), fast response time (25 s), high sensitivity (86 Ω/mg dL?1/cm?2) and a low value of the Michaelis‐Menten constant (Km, 0.8 mg/dL) with a regression coefficient of 0.997. 相似文献