Cloud point-magnetic solid phase extraction was used for the purpose of extraction and preconcentration of citalopram prior to its determination by the spectrofluorometric method. Non-ionic surfactant Triton X-100 was used for cloud point extraction and nickel zinc ferrite magnetic nanocomposite was used as a sorbent for the adsorption of surfactant rich phase. The implemented method involves initial extraction of the target analytes by CPE in the micelles of a non-ionic surfactant medium followed by using nickel zinc ferrite magnetic nanocom- posite to retrieve the micellar phase. Magnetic materials are then collected by applying an adscititious magnetic field to overcome the need for specific steps associated with CPE such as refrigeration of the condensed micellar phase to reduce its viscosity, centrifugation to separate the surfactant-rich phase and/or appropriate apparatus that enable direct sampling of the surfactant-rich phase. Under the optimal extraction conditions (i.e. pH: 9, ad- sorbent dosage: 60 mg, Triton X-100 concentration: 50 mg and t = 50 °C) the linear dynamic range and RSD were 3.00–800 ng mL −1 and 2.93%, respectively. A limit of detection of 0.42 ng mL −1 of citalopram was obtained for the method. Obtained results showed successful application of the method for the analysis of citalopram in the real samples.