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The sol-gel technology is applied for the preparation of three solid-phase microextraction (SPME) fibers for extracting of the volatile organic compounds (VOCs) from environmental water samples using gas chromatography-flame ionization detector (GC-FID).These fibers were prepared from different coating polymers including poly(dimethylsiloxane) (PDMS), poly(ethylene glycol) (PEG) and PEG reinforced with multi-walled carbon nanotubes (MWCNTs).