CMK-1 (carbon mesoporous from Korea) type ordered nanoporous carbon was investigated as a novel solid-phase microextraction fiber for the first time. The microextraction process was coupled with GC-FID and used to extract benzene, toluene, ethylbenzene and xylenes (BTEX) from the head space of the solution samples. Prepared fibers featured advantages like easy and fast preparation, high thermal and mechanical stability in which a fiber could be used for more than 60 tests. Employing Taguchi method and orthogonal array design; OA 16 (4 5 ), the HS-SPME of BTEX was optimized. Under the optimized conditions for all BTEX components, the linearity was from 3 to 800 lg L -1 , the relative standard deviation (RSD%) of the method was between 4.2 and 9.4% and limit of detections was between 0.27 and 1.1 lg L -1 . The recovery values were from 87.1 to 106.2% in water samples. Finally, the applicability of the proposed method was evaluated by the extraction and determination of BTEX in the water and petrochemical samples.

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