Herein we report on the synthesis, optimization of the synthetic procedure, functionalization, and characterization of cubic and spherical superparamagnetic magnetite nanoparticles. Spherical nanoparticles (16 ± 2 nm) were synthesized using oleylamine and oleic acid, and cubic (20 ± 2, 5 ± 0.5 nm) nanoparticles were synthesized with oleic acid and small amounts of oleylamine. Covalent modification of the nanoparticles was carried out using heterobifunctional PEG with aminopropyltriethoxysilane and N-hydroxysuccinimide ester moieties. This modification makes both water emulsion stability and further modification of the nanoparticles with cytotoxic drugs possible.