Preparation coating materials is the main point in solid-phase microextraction (SPME) fiber fabrications. So, fabricating MoS2 nanoflakes on graphenized HB (hard black) pencil lead was developed. The MoS2 nanoflakes were directionally arranged on graphenized HB pencil lead and used as a fiber coating for selectively headspace microextraction of phenolic compounds. The MoS2/graphenized pencil fibers were characterized by X-ray diffraction (XRD), field emission scanning microscopy (FESEM), thermal gravimetric analysis (TGA) and energy-dispersive X-ray spectroscopy (EDX).MoS2/graphenized pencil lead fibers indicated considerable potential due to extracting simultaneously trace amounts of some phenolic compounds in different water samples. The repeatabilities and detection limits for one fiber were between 5.5 and 7.2% and between 0.002 and 0.32 mgL1, respectability. The purpose method was a simple, quick, stable and cheap approach