A simple method has been developed for the preconcentration of benzene and phenolic compounds (BPC) by the adsorption of its carbon nanotubes (CNTs). The preconcentration of benzene and phenolic compounds (BPC) are ubiquitous pollutants, and many of them are carcinogenic or mutagenic. Carbon nanotubes (CNTs) are a kind of novel and interesting carbon material which can be used for separation and purification. In this investigation, commercial solid-phase microextraction (SPME) fibers (PDMS) were coated with single-wall nano tubes (SWNTs) and multi-wall nano tubes (MWNTs) to study the adsorption and extraction ability of hydrophobic BPC. While MWNTs adsorbed more hydrophobic BPC than SWNTs, the fibers coated with CNTs had advantages over traditional SPME fibers in selectivity and sensitivity. They could be used to separate hydrophobic BPC. The results show that the selectivity, sensitivity and reproducibility of this method are good for real sample analysis. Key words: Carbon nanotubes (CNTs), Solid-phase microextraction (SPME), preconcentration of benzene and phenolic compounds (BPC).