Preparation and biomedical application of layer-by-layer encapsulated oil in water magnetic emulsion

Hydrophilic submicron magnetic colloids were prepared via layer-by-layer encapsulation of oil in water (o/w) magnetic emulsions. The encapsulation explored in this work is based on sequential adsorption of oppositely charged polyelectrolytes onto magnetic emulsion. The functionalization was induced by the final polyelectrolyte layer. The elaborated magnetic particles were evaluated in the specific capture of nucleic acids.     

Preparation of biodegradable magnetic microspheres with poly(lactic acid)-coated magnetite

Poly(lactic acid) (PLA)-coated magnetic nanoparticles were made using uncapped PLA with free carboxylate groups. The physical properties of these particles were compared to those of oleate-coated or oleate/sulphonate bilayer (W40) coated magnetic particles. Magnetic microspheres (MMS) with the matrix material poly(lactide-co-glycolide) (PLGA) or PLA were then formed by the emulsion solvent extraction method with encapsulation efficiencies of 40%, 83% and 96% for oleate, PLA and oleate/sulfonate-coated magnetic particles, respectively. MMS made from PLA-coated magnetite were hemocompatible and produced no hemolysis, whereas the other MMS were hemolytic above 0.3 mg/mL of blood.     

The structuralization phenomena in magnetic fluid composites and their influence on transmissivity of light

A magnetic field induced agglomeration of magnetic and μm-sized copper non-magnetic particles in magnetic fluid with several volume concentrations of magnetite and copper particles was studied by means of optical microscope equipped with video camera. Transmission of light through two crossed polarizers and thin magnetic fluid and magnetic fluid composites film as a function of magnetic field was investigated. The experimental data showed that the presence of copper particles influences the aggregation processes of magnetic particles in magnetic fluids and transmissivity of light. Dedicated to Dr. Anton Zentko on the occasion of his 60th birthday. This work was supported by the Slovak Academy of Sciences within the framework of Project GAV No. 4001.     

Novel magnetic Fe onion-like fullerene micrometer-sized particles of narrow size distribution

Magnetic polydivinylbenzene (PDVB)/magnetite micrometer-sized particles of narrow size distribution were prepared by entrapping Fe(CO)₅ within the pores of uniform porous PDVB particles, followed by the thermal decomposition of the encapsulated Fe(CO)₅ at 300 °C in a sealed cell under inert atmosphere. Magnetic Fe onion-like fullerene micrometer-sized particles of narrow size distribution have been prepared by the thermal decomposition of the PDVB/magnetite magnetic microspheres at 1100 °C under inert atmosphere. The graphitic coating protects the elemental iron particles from oxidation and thereby preserves their very high magnetic moment for at least a year. Characterization of these unique magnetic carbon graphitic particles was also performed.     

Sonochemical synthesis of monodispersed magnetite nanoparticles by using an ethanol–water mixed solvent

The magnetite nanoparticles were synthesized in an ethanol–water solution under ultrasonic irradiation from a Fe(OH)₂ precipitate. XRD, TEM, TG, IR, VSM and UV/vis absorption spectrum were used to characterize the magnetite nanoparticles. It was found that the formation of magnetite was accelerated in ethanol–water solution in the presence of ultrasonic irradiation, whereas, it was limited in ethanol–water solution under mechanical stirring. The monodispersibility of magnetite particles was improved significantly through the sonochemical synthesis in ethanol–water solution. The magnetic properties were improved for the samples synthesized under ultrasonic irradiation. This would be attributed to high Fe²⁺ concentration in the magnetite cubic structure.     

Synthesis and characterization of magnetite particles covered with α-trietoxysilil-polydimethylsiloxane

New silicon magnetite ferrofluids were prepared by dispersing siloxane-coated magnetite particles in polydimethylsiloxane with low or high molecular weights. Ferrofluids are stable colloidal dispersions of ultra fine covered magnetite particles, which may be selected for a specific application. We demonstrated new methods of stabilizing the magnetic particles by reacting the hydroxyl groups on the surface of magnetite particles with terminal ethoxy groups of polydimethylsiloxane, followed by their dispersion in silicon fluids. The new silicon ferrofluids were tested from the morphology, magnetic properties/losses, and rheological properties point of view.     

Preparation and characterization of magnetic levan particles as matrix for trypsin immobilization

Magnetic levan was synthesized by co-precipitating D-fructofuranosyl homopolysaccharide with a solution containing Fe²⁺ and Fe³⁺ in alkaline conditions at 100 °C. The magnetic levan particles were characterized by scanning electron microscopy (SEM), magnetization measurements, X-ray diffractometry (XRD) and infrared spectroscopy (IR). Afterwards, magnetic levan particles were functionalized by NaIO₄ oxidation and used as matrices for trypsin covalent immobilization. Magnetite and magnetic levan particles were both heterogeneous in shape and levan-magnetite presented bigger sizes compared to magnetite according to SEM images. Magnetic levan particles exhibited a magnetization 10 times lower as compared to magnetite ones, probably, due to the coating layer. XRD diffractogram showed that magnetite is the dominant phase in the magnetic levan. Infrared spectroscopy showed characteristics absorption bands of levan and magnetite (O-H, C-O-C and Fe-O bonds). The immobilized trypsin derivative was reused 10 times and lost 16% of its initial specific activity only. Therefore, these magnetic levan particles can be proposed as an alternative matrices for enzyme immobilization.     

Preparation of improved catalytic materials for water purification

The aim of presented paper was to study preparation of catalytic materials for water purification. Iron oxide (Fe₃O₄) samples supported on activated carbon were prepared by wet impregnation method and low temperature heating in an inert atmosphere. The as-prepared, activated and samples after catalytic test were characterized by Mössbauer spectroscopy and X-ray diffraction. The obtained X-ray diffraction patterns of prepared samples show broad and low-intensity peaks of magnetite phase and the characteristic peaks of the activated carbon. The average crystallite size of magnetite particles was calculated below 20 nm. The registered Mössbauer spectra of prepared materials show a superposition of doublet lines or doublet and sextet components. The calculated hyperfine parameters after spectra evaluation reveal the presence of magnetite phase with nanosize particles. Relaxation phenomena were registered in both cases, i.e. superparamagnetism or collective magnetic excitation behavior, respectively. Low temperature Mössbauer spectra confirm this observation. Application of materials as photo-Fenton catalysts for organic pollutions degradation was studied. It was obtained high adsorption degree of dye, extremely high reaction rate and fast dye degradation. Photocatalytic behaviour of a more active sample was enhanced using mechanochemical activation (MCA). The nanometric size and high dispersion of photocatalyst particles influence both the adsorption and degradation mechanism of reaction. The results showed that all studied photocatalysts effectively decompose the organic pollutants under UV light irradiation. Partial oxidation of samples after catalytic tests was registered. Combination of magnetic particles with high photocatalytic activity meets both the requirements of photocatalytic degradation of water contaminants and that of recovery for cyclic utilization of material.     

External field-induced superferrimagnetism in magnetite nanoparticles

Film composites based on magnetite nanoparticles with a mean diameter of 4 nm in a polyvinyl alcohol matrix were studied by means of Mössbauer spectroscopy in a magnetic field of up to 3.4 kOe. The spectra were analyzed within the three-level relaxation model of the magnetic dynamics of an ensemble of single-domain particles, taking into account the precession and diffusion of the homogeneous magnetization of particles and their size distribution.     

Effect of surface treatment of magnetic particles on the preparation of magnetic polymer microspheres by miniemulsion polymerization

Surface treated magnetic particles were used to prepare well encapsulated submicron polystyrene/magnetic (PS/Fe₃O₄) composite microspheres via miniemulsion polymerization. The effects of the different surface treatment agents Disperbyk-106, Disperbyk-111, KH550, sodium dodecyl sulfate (SDS) and oleic acid were investigated on the encapsulation of polymer via miniemulsion polymerization. The interface interactions between magnetic particles, dispersants and coupling agents were analyzed from their IR spectra. It was found that Disperbyk-106 was the best dispersant in terms of preparing magnetic polymer microspheres with high encapsulation efficiency. The effect of wet or dry magnetic particles on encapsulation was also discussed.     

In vitro study of magnetic particle seeding for implant assisted-magnetic drug targeting

The concept of using magnetic particles (seeds) as the implant for implant assisted-magnetic drug targeting (IA-MDT) was analyzed in vitro. Since this MDT system is being explored for use in capillaries, a highly porous (ε∼70%), highly tortuous, cylindrical, polyethylene polymer was prepared to mimic capillary tissue, and the seeds (magnetite nanoparticles) were already fixed within. The well-dispersed seeds were used to enhance the capture of 0.87 μm diameter magnetic drug carrier particles (MDCPs) (polydivinylbenzene embedded with 24.8 wt% magnetite) under flow conditions typically found in capillary networks. The effects of the fluid velocity (0.015–0.15 cm/s), magnetic field strength (0.0–250 mT), porous polymer magnetite content (0–7 wt%) and MDCP concentration (C=5 and 50 mg/L) on the capture efficiency (CE) of the MDCPs were studied. In all cases, when the magnetic field was applied, compared to when it was not, large increases in CE resulted; the CE increased even further when the magnetite seeds were present. The CE increased with increases in the magnetic field strength, porous polymer magnetite content and MDCP concentration. It decreased only with increases in the fluid velocity. Large magnetic field strengths were not necessary to induce MDCP capture by the seeds. A few hundred mT was sufficient. Overall, this first in vitro study of the magnetic seeding concept for IA-MDT was very encouraging, because it proved that magnetic particle seeds could serve as an effective implant for MDT systems, especially under conditions found in capillaries.     

Core-shell structure and magnetic properties of magnetite magnetic fluids stabilized with dextran

The adsorption process of different dextran molecules onto the surface of in water dispersed magnetite nanoparticles has been investigated to optimize the preparation of magnetite magnetic fluids (MMFs). An average magnetite core size of 7.1 nm was found by X-ray diffraction and that of 8 nm was found by transmission electron microscopy for the samples prepared at 90 °C. An average hydrodynamic diameter of 25 nm was observed by scanning electron microscopy and that of 25-300 nm was obtained by photon correlation spectroscopy. The dextran was adsorbed by physical adsorption, a molecular weight of 20 kDa gave the best stability of these MMFs. The shell layer of the particles was weakly negatively charged in buffer solutions of pH values between 5.5 and 9.5. The particles seem to be mainly stabilized by sterical repulsion. The maximum available saturation magnetization of the MMFs was 3.5 kA/m.     

Physical and chemical properties of nanoscale magnetite-based solvent extractant

Nanoscale magnetite bearing magnetic carrier with an adsorbed layer of dibenzo-18-crown-6 was evaluated for removing radionuclides from nuclear waste solutions using magnetically assisted separation method. TEM results indicate that the average size of the base magnetite particles is ∼19 nm. The results of Mössbauer spectroscopy and field cooled (FC) and zero field cooled (ZFC) magnetization confirm the superparamagnetic behaviour of the magnetite particles in the polymer beads at room temperature and hence meet the requirement of magnetic filter regeneration capability.     

磁场下合成Fe3O4粉体的隧道磁阻

通过在半金属Fe₃O₄合成过程中外加磁场的方法，改变样品粒子的表面结晶状态和晶格缺陷，研究了由此引起的Fe₃O₄输运性质的变化.合成的Fe₃O₄粉体的主要导电机理均为自旋极化隧穿和高阶跃迁电导，电阻随温度升高成指数降低，电阻与电压显示了非线形相关性，磁阻与磁场的关系为蝴蝶形，是典型的隧道磁阻特征.与没有外加磁场时合成的样品比较，外加磁场合成的样品显示了更低的电阻和更高的磁阻.     

磁场下合成Fe3O4粉体的隧道磁阻

通过在半金属Fe₃O₄合成过程中外加磁场的方法,改变样品粒子的表面结晶状态和晶格缺陷,研究了由此引起的Fe₃O₄输运性质的变化.合成的Fe₃O₄粉体的主要导电机理均为自旋极化隧穿和高阶跃迁电导,电阻随温度升高成指数降低,电阻与电压显示了非线形相关性,磁阻与磁场的关系为蝴蝶形,是典型的隧道磁阻特征.与没有外加磁场时合成的样品比较,外加磁场合成的样品显示了更低的电阻和更高的磁阻. 关键词： 磁阻 隧穿 表面 晶格缺陷     

Quadrupole magnetic field-flow fractionation: A novel technique for the characterization of magnetic nanoparticles

Quadrupole magnetic field-flow fractionation (MgFFF) is an analytical separation and characterization technique for nano- and micro-sized magnetic particles. It fractionates particles according to their content of magnetite or other magnetic material. The potential and versatility of MgFFF for separation and characterization of magnetic nanoparticles, such as those used for immunospecific labeling of biological cells for magnetic separation, is demonstrated. A broadly polydisperse sample of dextran-coated magnetite nanoparticles was eluted under programmed field decay conditions, and quantitative data concerning the distribution of magnetite content were determined from the elution profile using a data reduction method.     

In situ hybridization to chitosan/magnetite nanocomposite induced by the magnetic field

Chitosan/magnetite nanocomposite was synthesized induced by magnetic field via in situ hybridization in ambient condition. Results of XRD patterns and TEM micrographs indicated that magnetite particles with 10–20 nm were dispersed in chitosan homogeneously. An interesting result is that magnetite nanoparticles were assembled to form chain-like structures under the influence of the external magnetic field, which mimics the magnetite chains inside of magnetotatic bacteria. The saturated magnetization (Ms) of nano-magnetite in chitosan was 50.54 emu/g, which is as high as 54% of bulk magnetite. The remanence (Mr) and coercivity (Hc) were 4 emu/g and14.8 Oe, respectively, which indicated that magnetite nanoparticles were superparamagnetic. The key of route is that a pre-precipitated chitosan hydrogel membrane, used as chemical reactor, which controlled the precipitation of chitosan precipitation and in situ transformation of magnetite from the precursor simultaneously in the magnetic field environment.