Trace amounts of pharmaceuticals and personal care products (PPCPs) are found in our water systems,and they are known to have adverse effects on wildlife and human at the ng/L to lg/L range, belowthe detection limit of most water analytical instruments. Methacrylate acid (MAA)-ethyl acrylate (EA)colloidal scaffolds were prepared via emulsion polymerization and used as templates for the in-situco-precipitation of Fe2+ to produce stable functional magnetic nanoparticles (MNPs) (<500 nm) decoratedwith b-cyclodextrin (b-CD) (FMNP). Emulsion polymerization with the controlled addition of monomermixtures allowed for good size control, and silica coating was introduced to prevent the oxidation ofFMNP. The superparamagnetic FMNP with high saturation magnetization (33 emu/g) could be readilyseparated from water using a high gradient magnetic separator (HGMS). Procaine hydrochloride (PrHy)was used as a model pharmaceutical residue to evaluate the performance of the FMNP, and 53.65 mgPrHy/g FMNP was absorbed using 600 ppm FMNP. A fast (30 min) adsorption kinetic follows thePseudo-first-order kinetic model that described the physical adsorption through a 1 to 1 host–guestinclusion mechanism. And the adsorption behavior followed the Freundlich isotherm with a linearadsorption performance. The proposed system is scalable and adaptable to existing water treatment processes,and it can be used for the detection of low concentration pharmaceuticals via a pre-concentratingstrategy.