Magnetic separation is a complex physical process in which magnetically susceptible composites is extracted from a liquid mixture using magnetic properties of the substances. Several separation procedures are developed based on magnetic susceptibility, magnetohydrostatic, magnetohydrodynamic and separation using eddy currents. The principle of separation by magnetic susceptibility consist different action of the magnetic force in competition with drag, gravity or friction forces. Within the separation by using magnetic susceptibility procedures the high-gradient magnetic separation (HGMS) is used to effectively separate magnetic materials from a nonmagnetic liquid medium. The HGMS techniques were applied to purify kaolin clay, the removal of iron particles from process streams in steel and power plants, desulphurize coal, wastewater treatment of bacteria and solids through magnetic seeding, organic substances and microorganisms. In the present report we describe a new nonhydrolytic single precursor route for the synthesis of polymer coated nickel ferrite superparamagnetic nanoparticles to separate soluble organic compounds for HGMS. Using nonhydrolytic techniques holds great potential for producing metal oxide nanoparticles with superior properties related to surface composition and defect structure.