Preparation coating materials is a fundamental point in solid-phase microextraction (SPME) fiber fabrications. So, a hydrothermal approach was developed for fabricating 3D hierarchically molybdenum disulfide/layered double hydroxide on anodized HB pencil lead, Nanosheets of a porous molybdenum disulfide and layered double hydroxide were directionally arranged on anodized HB pencil lead and used as a fiber coating for selectively analysis of polycyclic aromatic compounds (PAHs) by headspace SPME method. The assynthesized materials were characterized by thermal gravimetric analysis, scanning electron microscopy, and energy-dispersive X-ray spectroscopy, According to the results, this coating indicated considerable potential due to extracting trace amounts of some carcinogenic polycyclic aromatic compounds in water samples. The essential parameters such as extraction time, extraction temperature, agitation speed, and ionic strength of sample that mainly affect the adsorption process were optimized and in optimum values, the repeatabilities for one fiber were between 4.6% and 9.1% for the test compounds were achieved. The studied compounds were assessed within the detection limits as follows: 0.028 to 0.42 ngL1.
