Abstract: Melamine modified metal-organic framework (melamine-MOF) nanostructure was synthesized through the solvothermal method and used as sorbent for the micro-solid phase extraction (μ-SPE) of benzene, toluene, ethylbenzene and xylenes (BTEXs) from different types of water sample. The quantification was performed by gas chromatography-mass spectrometry (GC MS). The prepared sorbent was confirmed by different characterization including scanning electron microscopy (SEM), powdered X-ray diffraction (XRD), Brunauer Emmett Teller (BET) and Fourier transformed infrared (FT-IR) spectroscopy. Under the optimized condition, the method provided linearity range of between 0.5 and 500.0 μg L-1 (depending on the analytes) with good coefficients of determination (R2) ranging between 0.983 and 0.997. The relative standard deviations (RSDs) of the method for the analytes at 50 μg L-1 ranged from 5.5 to 11.8%