Based on solid phase extraction gas chromatography and mass spectrometry procedure for determining phenol and its derivatives in natural water was presented. In solid phase extraction, three types of techniques using solid phase adsorption material were applied, i.e. cartridge and disk extraction and solid-phase micro extraction. U.S. EPA 11 priority pollutant were treated with acid and salt, and converted second portion of acetyl derivatives. Under the these condition, extraction efficiency and detection ability dependent on extraction methods were discussed. Obtained results using optimized solid phase extraction techniques showed more convenience, simplifier and lower cost than the conventional analytical methods with holding wide dynamic range and lower detection limits.