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.     

Synthesis of magnetite nanoparticles for AC magnetic heating

Magnetite particles with different average diameter (D_m) suitable for magnetic fluid hyperthermia (MFH) were synthesized by controlled coprecipitation technique. In this method, the reaction pH was stabilized using the pH buffer and the average particle diameter decreased with increasing reaction pH. The size-dependent magnetic behavior of the magnetite nanoparticles was studied and the optimum size range required for magnetic fluid hyperthermia (MFH) has been arrived at. Among the samples studied, the maximum specific absorption rate of 15.7 W/g was recorded for the magnetite sample with D_m of 13 nm, when exposed to an AC magnetic field strength of 3.2 kA/m and a frequency of 600 kHz. The AC magnetic properties suggested that the size distribution of the sample was bimodal with average particle size less than ∼13 nm.     

Preparation and application of magnetic poly(styrene-glycidyl methacrylate) microspheres

A novel method for the preparation of polymer-based, magnetic microspheres is proposed. Pre-made, poly(styrene-glycidyl methacrylate) (PS-GMA) particles of micron size were swollen by a mixture of N-methyl-2-pyrrolidone and water, and then incubated with superparamagnetic nanoparticles. The nanoparticles were allowed to diffuse into polymer microspheres during the incubation, became entrapped and made the polymer microspheres superparamagnetic. These magnetic PS-GMA microspheres were chemically modified and then coupled with single-stranded oligonucleotides as probes for DNA hybridization. The immobilized probes showed repeatable capture of target oligonucleotides.     

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.     

Preparation of magnetic composite microspheres by surfactant free controlled radical polymerization: Preparation and characteristics

Submicron magnetic composite microspheres have been prepared by a new surfactant free controlled radical polymerization. This new approach is based on the use of diphenylethene (DPE) as radical controlling agent and no emulsifier is required. X-ray powder diffraction (XRD), thermogravimetric analysis (TGA) and transmission electron microscopy (TEM), etc. were conducted to characterize the magnetite particles and magnetic composite microspheres. The average size of the magnetic composite microspheres prepared by this new approach is 265 nm and the magnetite content of the composite microspheres is around 20%. Furthermore, the magnetic composite microspheres which surfaces have epoxy groups were also prepared.     

A microfluidic spiral for size-dependent fractionation of magnetic microspheres

Magnetic microspheres (MMS) are useful tools for a variety of medical and pharmaceutical applications. Typically, commercially manufactured MMS exhibit broad size distributions. This polydispersity is problematic for many applications. Since the direct synthesis of monodisperse MMS is often fraught with technical challenges, there is considerable interest in and need associated with the development of techniques for size-dependent fractionation of MMS. In this study we demonstrated continuous size-dependent fractionation of sub-micron scale particles driven by secondary (Dean effect) flows in curved microfluidic channels. Our goal was to demonstrate that such techniques can be applied to MMS containing superparamagnetic nanoparticles. To achieve this goal, we developed and tested a microfluidic chip for continuous MMS fractionation. Our data address two key areas. First, the densities of MMS are typically in the range 1.5–2.5 g/cm³, and thus they tend be non-neutrally buoyant. Our data demonstrate that efficient size-dependent fractionation of MMS entrained in water (density 1 g/cm³) is possible and is not significantly influenced by the density mismatch. In this context we show that a mixture comprising two different monodisperse MMS components can be separated into its constituent parts with 100% and 88% success for the larger and smaller particles, respectively. Similarly, we show that a suspension of polydisperse MMS can be separated into streams containing particles with different mean diameters. Second, our data demonstrate that efficient size-dependent fractionation of MMS is not impeded by magnetic interactions between particles, even under application of homogeneous magnetic fields as large as 35 kA/m. The chip is thus suitable for the separation of different particle fractions in a continuous process and the size fractions can be chosen simply by adjusting the flow velocity of the carrier fluid. These facts open the door to size dependent fractionation of MMS.     

超声耦合用磁性液体的研究

磁性液体可作为一种新型超声耦合剂，作者通过合理选择磁性液体的组分，改进其制备工艺，研制出吸附性强，流失损耗小，透声性好的两种磁性液体，它们在超声检测中具有独特的优点。     

Preparation and magnetic properties of magnetite nanoparticles by sol–gel method

 Magnetite (Fe₃O₄) nanoparticles have been successfully synthesized by sol–gel method combined with annealing under vacuum. The phase structures, morphologies, particle sizes, chemical composition, and magnetic properties of Fe₃O₄ nanoparticles have been characterized by X-ray diffraction, field emission scanning electron microscopy, energy-dispersive X-ray spectrometer and vibrating sample magnetometer (VSM). The results indicate that the size, the corresponding saturation magnetization value and coercivity value of Fe₃O₄ nanoparticles increase with the increase of synthesized temperature. And the phase transformation of Fe₃O₄ nanoparticles has been studied under different atmospheres and temperatures.     

Study on immobilization of lipase onto magnetic microspheres with epoxy groups

Magnetic microspheres were synthesized by the suspension polymerization of glycidyl methacrylate (GMA), methacrylic acid (MAA) and divinyl benzene (DVB) in the presence of oleic acid-coated Fe₃O₄ nanoparticles. Triacylglycerol lipase from porcine pancreas was covalently immobilized on the magnetic microspheres via the active epoxy groups with the activity yield up to 63% (±2.3%) and enzyme loading of 39 (±0.5) mg/g supports. The resulting immobilized lipase had higher optimum temperature compared with those of free lipase and exhibited better thermal, broader pH stability and excellent reusability. Furthermore, the catalyzed capability of immobilized lipase was also investigated by catalyzing synthesis of hexyl acetate and the esterification conversion rate reached to 83% (±2.5%) after 12 h in nonaqueous solvent.     

A novel approach to preparing magnetic protein microspheres with core-shell structure

Magnetic protein microspheres with core-shell structure were prepared through a novel approach based on the sonochemical method and the emulsion solvent evaporation method. The microspheres are composed of the oleic acid and undecylenic acid modified Fe₃O₄ cores and coated with globular bovine serum albumin (BSA). Under an optimized condition, up to 57.8 wt% of approximately 10 nm superparamagnetic Fe₃O₄ nanoparticles could be uniformly encapsulated into the BSA microspheres with the diameter of approximately 160 nm and the high saturation magnetization of 38.5 emu/g, besides of the abundant functional groups. The possible formation mechanism of magnetic microspheres was discussed in detail.     

Preparation and characterization of biodegradable magnetic carriers by single emulsion-solvent evaporation

This paper describes a single emulsion-solvent evaporation protocol to prepare PEGylated biodegradable/biocompatible magnetic carriers by utilizing hydrophobic magnetite and a mixture of poly(D,L lactide-co-glycolide) (PLGA) and poly(lactic acid-block-polyethylene glycol) (PLA-PEG) (26:1 by mass) polymers. We characterized the magnetic microspheres in terms of morphology, composite microstructure, size and size distribution, and magnetic properties. Results show that the preparation produces magnetic microspheres with a good spherical morphology, small size (mean diameter of 1.2–1.5 μm) by means of large size distributions, and magnetizations up to 20–30 emu/g of microspheres.     

Preparation of magnetic polylactic acid microspheres and investigation of its releasing property for loading curcumin

In order to obtain a targeting drug carrier system, magnetic polylactic acid (PLA) microspheres loading curcumin were synthesized by the classical oil-in-water emulsion solvent-evaporation method. In the Fourier transform infrared spectra of microspheres, the present functional groups of PLA were all kept invariably. The morphology and size distribution of magnetic microspheres were observed with scanning electron microscopy and dynamic light scattering, respectively. The results showed that the microspheres were regularly spherical and the surface was smooth with a diameter of 0.55-0.75 μm. Magnetic Fe₃O₄ was loaded in PLA microspheres and the content of magnetic particles was 12 wt% through thermogravimetric analysis. The magnetic property of prepared microspheres was measured by vibrating sample magnetometer. The results showed that the magnetic microspheres exhibited typical superparamagnetic behavior and the saturated magnetization was 14.38 emu/g. Through analysis of differential scanning calorimetry, the curcumin was in an amorphous state in the magnetic microspheres. The drug loading, encapsulation efficiency and releasing properties of curcumin in vitro were also investigated by ultraviolet-visible spectrum analysis. The results showed that the drug loading and encapsulation efficiency were 8.0% and 24.2%, respectively. And curcumin was obviously slowly released because the cumulative release percentage of magnetic microspheres in the phosphate buffer (pH=7.4) solution was only 49.01% in 72 h, and the basic release of curcumin finished in 120 h.     

Fast fabrication of epoxy-functionalized magnetic polymer core-shell microspheres using glycidyl methacrylate as monomer via photo-initiated miniemulsion polymerization

Epoxy-functionalized magnetic polymer microspheres with high magnetic responsiveness were prepared through a one-step photo-initiated miniemulsion polymerization. This kind of core-shell particle can be synthesized successfully with hydrophilic monomer, glycidyl methacrylate, as a single monomer by a 10 min ultraviolet irradiation, and phase separation induced eccentric cores. The morphology of the particles was examined with a transmission electron microscope and a scanning electron microscope. The incorporation of magnetic particles was characterized with X-ray diffraction. The magnetic content of the microspheres was detected by both vibrating sample magnetometer and thermo-gravimetric analyzer.     

Synchronous ultrasonic Doppler imaging of magnetic microparticles in biological tissues

We considered applicability of acoustic imaging technology for the detection of magnetic microparticles and nanoparticles inside soft biological tissues. Such particles are widely used for magnetically targeted drug delivery and magnetic hyperthermia. We developed a new method of ultrasonic synchronous tissue Doppler imaging with magnetic modulation for in vitro and in vivo detection and visualization of magnetic ultradisperse objects in soft tissues. Prototype hardware with appropriate software was produced and the method was successfully tested on magnetic microparticles injected into an excised pig liver.     

Application of magnetic poly(styrene-glycidyl methacrylate) microspheres for immunomagnetic separation of bone marrow cells

Surface-functionalized magnetic poly(styrene-glycidyl methacrylate) (PS-GMA) microspheres were prepared and coupled with Sca-1 antibody for cell selection from murine bone marrow mononuclear cells (MNCs). Biotinylated Sca-1 antibody could be directly coupled to avidin-bound magnetic microspheres. Alternatively, oxidized goat anti-mouse antibody was covalently bound onto the amino group-containing magnetic microspheres in a site-directed manner, and the resultant conjugate was coupled with non-modified Sca-1 antibody. Using the indirect antibody-bound magnetic microspheres, the purity of isolated Sca-1⁺ cells increased with bead-to-cell ratio. Using a bead-to-cell ratio of 10 beads/cell, a purity of 85% Sca-1⁺ cells corresponding to a 17-fold enrichment was achieved.     

Synthesis and characterization of noscapine loaded magnetic polymeric nanoparticles

The delivery of noscapine therapies directly to the site of the tumor would ultimately allow higher concentrations of the drug to be delivered, and prolong circulation time in vivo to enhance the therapeutic outcome of this drug. Therefore, we sought to design magnetic based polymeric nanoparticles for the site directed delivery of noscapine to invasive tumors. We synthesized Fe₃O₄ nanoparticles with an average size of 10±2.5 nm. These Fe₃O₄ NPs were used to prepare noscapine loaded magnetic polymeric nanoparticles (NMNP) with an average size of 252±6.3 nm. Fourier transform infrared (FT-IR) spectroscopy showed the encapsulation of noscapine on the surface of the polymer matrix. The encapsulation of the Fe₃O₄ NPs on the surface of the polymer was confirmed by elemental analysis. We studied the drug loading efficiency of polylactide acid (PLLA) and poly (l-lactide acid-co-gylocolide) (PLGA) polymeric systems of various molecular weights. Our findings revealed that the molecular weight of the polymer plays a crucial role in the capacity of the drug loading on the polymer surface. Using a constant amount of polymer and Fe₃O₄ NPs, both PLLA and PLGA at lower molecule weights showed higher loading efficiencies for the drug on their surfaces.     

Stability of the magnetic domain structure of nanoparticle thin films against external fields

We investigate the effect of external magnetic fields on the magnetic structure of thin films from magnetic nanoparticles (MNP) with dipolar interaction. Such fields are present, for example, if samples are scanned with magnetic probes. Numerical simulations and experimental magnetic force microscopy (MFM) studies are presented. Numerically, we have calculated the magnetization pattern of single-layer and multilayer MNP thin films. The calculations show that unperturbed single-layer MNP films have an in-plane orientation of the magnetization with a flux-closure-domain pattern. An external field generated by a point dipole above the film induces locally an out-of-plane configuration of the magnetization. In the corresponding MFM images, the domain pattern in the film is erased and a stripe-like contrast enhancement at the edges appears. Multilayer films are found to be more robust against external fields than monolayers.     

Heating of magnetic fluid systems driven by circularly polarized magnetic field

A theory is presented to calculate the heat dissipation of a magnetic suspension, a ferrofluid, driven by circularly polarized magnetic field. Theory is tested by in vitro experiments and it is shown that, regardless of the character of the relaxation process, linearly and circularly polarized magnetic field excitations, having the same root-mean-square magnitude, are equivalent in terms of heating efficiency.     

Synthesis of copper-nickel nanoparticles prepared by mechanical milling for use in magnetic hyperthermia

Mechanical alloying of a mixture of copper and nickel powders has been applied for the preparation of copper-nickel alloy particles in the nanometer range. The particles were designed to be used for controlled magnetic hyperthermia applications. The milling conditions were optimized using the desired alloy composition. Utilizing a ball-to-powder mass ratio of 20, we could obtain a nanocrystalline Cu_27.5Ni_72.5 (at%) alloy with a crystallite size of around 10 nm and a Curie temperature of 45 °C.Thermal demagnetization in the vicinity of the Curie temperature of the nanoparticles was determined by thermomagnetic measurements using an adapted TGA-SDTA apparatus. The size and morphology of the particles were determined by XRD measurements and TEM analyses. The magnetic properties were also examined with a VSM. The magnetic heating effects were measured for the powdered material.     

Application of superparamagnetic microspheres for affinity adsorption and purification of glutathione

The superparamagnetic poly-(MA–DVB) microspheres with micron size were synthesized by the modified suspension polymerization method. Adsorption of glutathione by magnetic poly-(MA–DVB) microspheres with IDA-copper was investigated. The effect of solution pH value, affinity adsorption and desorption of glutathione was studied. The results showed that the optimum pH value for glutathione adsorption was found at pH=3.5, the maximum capacity for glutathione of magnetic poly-(MA–DVB) microspheres was estimated at 42.4 mg/g by fitting the experimental data to the Langmuir equation. The adsorption equilibrium of glutathione was obtained in about 10 min and the adsorbed glutathione was desorbed from the magnetic microspheres in about 30 min using NaCl buffer solution. The magnetic microspheres could be repeatedly utilized for the affinity adsorption of glutathione.