The main goal of this study is the hierarchical synthesis nano structure MnO2/NiCo2S4 on the graphenized pencil lead and application as solid phase microextraction fiber for mensuration of polycyclic aromatic hydrocarbons in surface water samples. In this study, MnO2/NiCo2S4/GPL fiber was synthesized by hydrothermal method and characterized by EDX, SEM and FT-IR. Then its extraction efficiency for polycyclic aromatic hydrocarbons (PAHs) in surface water samples via the HS-SPME method was evaluated. The results revealed that prepared fiber is appropriate for quantitative determination. Identification of desorbed analytes from the surface of fiber was performed in combination GC-FID. Under the optimized conditions, the linear response for the analytes was observed in the range from 0.0001 to 100 mgL1 with the correlation coefficients (R2) ranged from 0.994 to 0.998 and the limits of detection (LOD) between 0.3 and 0.05 ngL1. The proposed fiber was successfully used for the determination of polycyclic aromatic hydrocarbons spiked in surface water samples and RSD% values were obtaine in the range of 8.4 9.8%
