A simple dispersive solid-phase micro-extraction method based on CoFe2O4 nano-particles (NPs) functionalized with 8-hydroxyquinoline (8-HQ) with the aid of sodium dodecyl sulfate (SDS) was developed for separation of Al(III) ions from aqueous solutions. Al(III) ions are separated at pH 7 via complex formation with 8-HQ using the functionalized CoFe2O4 nano-particles sol solution as a dispersed solid-phase extractor. The separated analyte is directly quantified by a spectrofluorometric method at 370nm excitation and 506nm emission wavelengths. A comparison of the fluorescence of Al(III)-8-HQ complex in bulk solution and that of Al(III) ion interacted with 8-HQ/SDS/CoFe2O4 NPs revealed a nearly 5-fold improvement in intensity. The experimental factors influencing the separation and in situ monitoring of the analyte were optimized. Under these conditions, the calibration graph was linear in the range of 0.1-300ngmL(-1) with a correlation coefficient of 0.9986. The limit of detection and limit of quantification were 0.03ngmL(-1) and 0.10ngmL(-1), respectively. The inter-day and intra-day relative standard deviations for six replicate determinations of 150ngmL(-1) Al(III) ion were 2.8% and 1.7%, respectively. The method was successfully applied to direct determine Al(III) ion in various human serum and water samples.