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Synthesis a well-suited coating for solid phase microextraction (SPME) fiber is essential point due to determination trace amounts of analytes from water and wastewater samples. So, the new coating was built onto the porous anodized aluminum wire incorporated with layered double hydrox-ide compound and modified solvothermally with graphitic carbon nitride and used as fiber coating for selectively analysis of polycyclic aromatic hydrocarbons by HS-SPME method. According to the results, this coating indicated considerable potential due to extract simultaneously trace amounts of some carcinogenic polycyclic aromatic compounds in different matrices. Essential parameters such as microextraction time, microextrac-tion temperature, agitation speed and ionic strength of the sample solu-tion that mainly affect the adsorption process were optimized and in the optimum values, repeatability data of one fiber that changed between 4.7% and 7.7% for the test compounds were achieved. Detection limits for the studied compounds were between 0.002 to 0.32mgL
1 . It is a simple, quick, and cheap approach. There is stability in the fiber in terms of tem-perature, and great recoveries are obtained by its use.