This workreportsonamethodforselectiveextractionandsensitivedeterminationofamoxicillindrug (AMX). ThemethodisbasedonsolidphaseextractionofAMXbyanovelmodified magneticna- noadsorbent priortospectrophotometricdeterminationofAMXusingaprocedurebasedonformationa colored azo-derivativeoftheinvestigateddrug.Thenanoadsorbenthasbeensynthesizedbymodification ofmagnetic-multiwalledcarbonnanotubewithdibenzo-18-crown-6moieties.Thesynthesized nanoparticles werecharacterizedusingTEM,XRDandFT-IRmeasurements.Atthenextstep,various factors thatcouldpotentiallyaffectadsorptionanddesorptionefficiencies ofAMX,havebeenoptimized. The resultsshowedthatundertheoptimizedconditions,sensitiveandselectivedeterminationofthe investigateddruginconcentrationrangeof5.0–1000.0ngmL1 with thelimitofdetectionof 3.0 ngmL1 wasachievable.Furthermore,therealsampleanalysis(i.e.amoxicillincapsulesandhuman urine samples)resultsindicatedthatareliablepromisingcandidatemethodhasbeendevelopedforthe determination ofAMXintheinvestigatedrealsamples.