Mesoporous materials were employed as fast, sensitive and efficient fiber coatings of solid-phase microextraction (SPME) for the first time. Three micrometer as-synthesized C-16-MCM-41 particles were immobilized onto stainless steel wire with 100 mum coating thickness. In combination with high performance liquid chromatography (HPLC), extraction efficiency and selectivity Of C-16-MCM-41 were investigated using aromatic hydrocarbons. Effect of extraction and desorption time, extraction temperature, stirring rate and ionic strength on extraction efficiency were examined. Aanalytical merits of SPME with C-16-MCM-41 coating were evaluated. The chromatographic peak area is proportional to the concentration of anthracene in the range 0.5-150 mug l(-1). The limit of detection was 0.05 mug l(-1) (S/N = 3) and the relative standard deviation (R.S.D.) was 0.033%. (C) 2003 Elsevier B.V. All rights reserved.