Well Defined Poly(Methyl Methacrylate)-Fe3O4/Poly(Vinyl Pivalate) Core-Shell Superparamagnetic Nanoparticles: Design and Evaluation of In Vitro Cytotoxicity Activity Against Cancer Cells.

The objective of this work is to develop and characterize polymeric nanoparticles with core-shell morphology through miniemulsion polymerization combined with seeded emulsion polymerization, aiming at the application in the treatment of vascular tumors via intravascular embolization. The synthesis of the core-shell nanocomposites was divided into two main steps: (i) Formation of the core structure, consisting of poly(methyl methacrylate)/magnetic oxide coated with oleic acid (OM-OA) via miniemulsion and (ii) shell structure produced through seeded emulsion polymerization of vinyl pivalate. Nanocomposites containing about 8 wt.% of OM-OA showed high colloidal stability, mean diameter of 216.8 nm, spherical morphology, saturation magnetization (Ms) of 4.65 emu·g-1 (57.41 emu·g-1 of Fe3O4), preserved superparamagnetic behavior and glass transition temperature (Tg) of 111.8 °C. TEM micrographs confirmed the obtaining of uniformly dispersed magnetic nanoparticles in the PMMA and that the core-shell structure was obtained by seeded emulsion with Ms of 1.35 emu·g-1 (56.25 emu·g-1 of Fe3O4) and Tg of 114.7 °C. In vitro cytotoxicity assays against murine tumor of melanoma (B16F10) and human Keratinocytes (HaCaT) cell lines were carried out showing that the core-shell magnetic polymeric materials (a core, consisting of poly(methyl methacrylate)/Fe3O4 and, a shell, formed by poly(vinyl pivalate)) presented high cell viabilities for both murine melanoma tumor cell lines, B16F10, and human keratinocyte cells, HaCaT.

Estimating mean crystallite size of magnetite using multivariate calibration and powder x-ray diffraction analysis.

Powder X-ray diffraction patterns for 29 samples of magnetite, acquired using a conventional diffractometer, were used to build PLS calibration-based methods and variable selection to estimate mean crystallite size of magnetite directly from powder X-ray diffraction patterns. The best IPLS model corresponds to the Bragg reflections at 35.4° (h k l = 3 1 1), 43.0° (h k l = 4 0 0), 53.6° (h k l = 4 2 2), and 57.0° (h k l = 5 1 1) in 2θ. The best model was a GA-PLS which produced a model with RMSEP of 0.9 nm, and a correlation coefficient of 0.9976 between mean crystallite sizes calculated using Williamson-Hall approach and the ones predicted by GA-PLS method. These results indicate that magnetite mean crystallite sizes can be predicted directly from Powder X-Ray Diffraction and multivariate calibration using PLS variable selection approach.