For specific applications in the field of high gradient magnetic separation of biomaterials, magnetic nanoparticle clusters of controlled size and high magnetic moment in an external magnetic field are of particular interest. We report the synthesis and characterization of magnetic microgels designed for magnetic separation purposes, as well as the separation efficiency of the obtained microgel particles. High magnetization magnetic microgels with superparamagnetic behaviour were obtained in a two-step synthesis procedure by a miniemulsion technique using highly stable ferrofluid on a volatile nonpolar carrier. Spherical clusters of closely packed hydrophobic oleic acid-coated magnetite nanoparticles were coated with cross linked polymer shells of polyacrylic acid, poly-N-isopropylacrylamide, and poly-3-acrylamidopropyl trimethylammonium chloride. The morphology, size distribution, chemical surface composition, and magnetic properties of the magnetic microgels were determined using transmission electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. Magnetically induced phase condensation in aqueous suspensions of magnetic microgels was investigated by optical microscopy and static light scattering. The condensed phase consists of elongated oblong structures oriented in the direction of the external magnetic field and may grow up to several microns in thickness and tens or even hundreds of microns in length. The dependence of phase condensation magnetic supersaturation on the magnetic field intensity was determined. The experiments using high gradient magnetic separation show high values of separation efficiency (99.9-99.97%) for the magnetic microgels.

The synthesis and characterization of hybrid structures obtained by coating Fe3O4 magnetic nanoparticles from water based nanofluid with a polypyrrole (PPy) layer are reported. The thin amorphous layer of polypyrrole surrounding the crystalline magnetic core was observed by HRTEM. The FTIR spectra of the nanocomposites show that the absorption bands characteristic for pyrrole ring vibrations significantly shifted to lower frequencies in the nanocomposite spectra, which indicates a higher degree of oxidation of the PPy shell covering the magnetite as compared with conventional PPy. The existence of superparamagnetism in the investigated nanocomposites is evidenced by the missing hysterezis loop in the magnetization versus applied magnetic field dependences. The comparison between the physical size of nanoparticles determined from TEM analysis and the magnetic size deduced from magnetization measurements is discussed. The surface modification of magnetite by polypyrrole coating results in an increase in the saturation magnetization and of the apparent magnetic diameter of the nanoparticles. This novel effect is attributed to a charge transfer process from the conducting polymer to the surface iron ions of magnetite, producing an increase in the surface contribution to the overall magnetic moment of the nanoparticles.

The graft polymerization of e-caprolactone (e-CL) onto magnetite was carried out under microwave irradiation in the presence of tin(II) 2-ethylhexanoate. The molar ratio of e-CL to tin(II) 2-ethylhexanoate was 300, whereas the molar ratio of e-CL to magnetite was 5. The chemical structures of the obtained poly(e-caprolactone) coated magnetic nanoparticles were characterized by FTIR and XPS spectroscopy. These magnetic-polymer hybrid nanostructures were further investigated by X-ray diffraction and magnetization measurements. The morphology of the magnetic core-shell nanostructures were determined by TEM.

Dental adhesives are used in a wide range of applications, including to place direct composite restorations in frontal or posterior teeth. One of the most frequent causes for the failure of composite resin restorations is microleakages. The first aim of this work is to introduce a new type of self-etched dental adhesive doped with magnetic nanoparticles (MPs) synthetized in the laboratory. The scope is to produce adhesives with a minimized width/thickness to decrease the risk of microleakages. The second aim is to assess the width/thickness of the adhesive layer in all the characteristic areas of the teeth using both the less precise but most common optical microscopy and the more accurate and volumetric micro-Computed Tomography (CT) investigations. Twenty extracted teeth have been divided into four groups: Group 1 includes ‘blank’ samples with adhesives that are not doped with MPs; Group 2 includes samples with adhesives doped with MPs; Groups 3 and 4 include samples with adhesives doped with MPs that are subjected to an active magnetic field for 5 and 10 min, respectively. Microscopy investigations followed by micro-CT and EDAX are performed on the adhesive. While a rather good agreement is obtained between the microscopy and micro-CT results, the capability of the latter to offer a full volumetric reconstruction of the layer is exploited to analyze the adhesion of the four considered dental materials. Thus, from micro-CT results the graphs of the surface areas as functions of the adhesive layer width are modeled mathematically, as well as the volume of sealants, for each of the four groups. To our knowledge, it is the first time that such a methodology is used. Characteristic parameters are extracted and the ascertainment of the optimal parameter that should be utilized for such assessments is discussed. The study demonstrates the adhesion improvement produced for Groups 3 and 4, where MPs are used. It also concludes that the magnetic field should be applied to the adhesive material for the longest possible exposure time (with a trade-off with the clinical duration of the treatment).

Magnetoresponsive microgels with high saturation magnetization values have been obtained by a strategy based on the miniemulsion method using high colloidal stability organic carrier ferrofluid as primary material. Hydrophobic nanoparticles Fe 3 O 4 /oleic acid are densely packed into well-defined spherical nanoparticle clusters coated with polymers with sizes in the range 40-350 nm. Physical-chemical characteristics of magnetic microgels were investigated by TEM, SAXS, XPS and VSM measurements with the focus on the structure-properties relationship. The impact of magnetic microgels loaded with anticancer drug mitoxantrone (MTO) on the nonadherent human T cell leukemia line Jurkat was investigated in multiparameter flow cytometry. We showed that both MTO and microgel-loaded MTO penetrate into cells and both induce apoptosis and later secondary necrosis in a time-and dose dependent manner. In contrast, microgels without MTO are not cytotoxic in the corresponding concentrations. Our results show that MTO-loaded microgels are promising structures for application in magnetic drug targeting.

Magnetite (Fe3O4) and ferrite (MFe2O4, M = Mn, Zn) hydrophobic magnetic nanoparticles with various shapes and sizes were synthesized by high-temperature reaction of organic precursor solutions. Spherical, cubic, hexagonal, and octahedral shapes and sizes ranging from 10 to 100 nm were obtained. It has been proven that the reported high capability of tailoring the shape and the size of the surface-coated nanoparticles allows controlling a variety of properties that are relevant to many potential applications. Structurally well-formed hydrophobic magnetic nanoparticles with high saturation magnetization values are reported. The hydrophobic oleic acid shell was successfully transformed by a simple and environmentally friendly oxidative scission method into azelaic acid. The morphostructural characteristics, size distributions, chemical composition, and magnetic properties of the resulting hydrophilic nanoparticles were investigated by electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, Mössbauer spectroscopy, superconducting quantum interference device, and vibrating sample magnetometry. Magnetic hyperthermia measurements have been performed in a specially designed sample holder placed in an inductor with copper windings assuring alternating magnetic fields of safely biological amplitude-frequency products. The optimal shape with a specific size range for nanoparticles dispersed in various carriers providing the best heating efficiency is reported.

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