A simple and sensitive analytical procedure by solid-phase extraction method combined with high-performance liquid chromatography and using of graphene-magnetite nanomaterials as sorbent has been developed for the determination of atorvastatin in human plasma. A magnetic solid-phase extraction method as a simple, fast, and efficient extraction technique has been used for sample preparation. A solid nanocomposite material, graphene nanosheets decorated with magnetite nanoparticles, was used as a magnetic adsorbent and the adsorption process was optimized in this study. RP C18 column was used with mobile phase composed of acetonitrile-10mM orthophosphoric acid by isocratic elution with the flow rate of 1mLmin(-1). Fluorimetric detection was used by the excitation wavelength at 282nm and the emission wavelength at 400nm. It was found that the calibration curve was linear in the 30-150ngmL(-1). Limit of detection and limit of quantitation values were found to be 10 and 30ngmL(-1), respectively. The intra-day and inter-day relative standard deviation values were less than 5.27%. It has been concluded that the new developed method provides fast, simple, cost reduced, and sensitive assay for atorvastatin determination in human plasma. This method is also applied to a pharmacokinetic study.