In this work, the synthesized Fe 3 O 4 nanoparticles was coated by sodium dodecyl sulfate and then it was used as a sorbent in mixed-hemimicelle solid phase extraction of some amphetamines, as psychoactive drugs, from biological samples. This extraction method was combined with dispersive liquid-liquid microextraction to enhance enrichment factors of targeted analytes. Effect of different parameters influencing the hybrid extraction performance, such as sodium dodecyl sulfate amount and sample pH, were investigated. The method showed linearity in the range of 1.0-250 and 2.0-250 µg L -1 for the most of analytes in urine and plasma samples, respectively. The limits of detection, based on signal to noise of 3, were found 0.1-0.2 and 0.3-0.5 µg L -1 in urine and plasma samples, respectively. The results of the intra-day and inter-day precision were less than 13.5% for all amphetamines. The amounts of relative recoveries in spiked urine and plasma samples were found in the range of 90-96 and 87-93%, respectively.