A solid phase extraction (SPE) and high-performance liquid Chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) method was developed and validated for qualitative and quantitative determination of fluoroquinolone (FQ) compounds in milk samples. The FQ compounds were: ofloxacin, norfloxacin and ciprofloxacin. Extraction of FQs was carried out using two types of sorbents: magnetic nano particles (MNP) and styrene divinyl benzene co-polymer. Two types of MNP were used including: graphene magnetite (GM) and graphene oxide magnetite (GOM). Results showed that styrene divinyl benzene co-polymer gives high recoveries (85-100%) with optimum condition for the extraction of the three analytes using elution solvent 90:10 % of ACN: MeOH. The optimum mobile phase used consist of solvent A 0.1% formic acid and methanol as solvent B (75:25). Moreover, MS/MS conditions were optimized in positive modes. Multiple reaction-monitoring modes (MRM) were used to determined precursor ion and product ions of the FQs compounds. The developed method was validated. The linear regression (R2 ) ranged between 0.996 and 0.997 while the limit of detection (LOD) was between 0.0032 and 0.016 ng mL-1 . Finally, milk samples purchased from the local market were analyzed and results showed low traces of FQs compounds are presents in these samples.