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Citrinin (CIT) is a mycotoxin naturally in many foods that causes carcinogenic and mutagenic effects in the human body. A novel method was developed for the selective quantification of citrinin in rye samples. Citrinin-imprinted spheres were fabricated through reversible addition fragmentation chain transfer (RAFT) precipitation polymerization (RAFTPP) in the presence of 2-hydroxymethacrylate (HEMA, functional monomer), ethylene glycol dimethacrylate (EGDMA, cross-linker), citrinin (template), 4-cyano-4-(phenylcarbonothioylthio)pentanoic acid (CTA, RAFT agent), azobisisobutyronitrile (AIBN, initiator), and acetonitrile (ACN, porogen). The imprinted polymers were shown to be spherical with a high surface area and a porous structure. The rebinding properties of citrinin to the imprinted spheres were also examined in detail. The maximum adsorption capacity, equilibration time, and imprinting factor were 38.6 …