In the present work experimental conditions were optimized for the analysis of organochlorine traces in water matrix using solid-phase microextraction (SPME) followed by gas chromatography with mass selective detector. The parameters including time of exposure of the fiber in the aqueous sample, fiber type, agitation speed, pH, ionic forces, temperature of adsorption, and time of desorption were evaluated. The best conditions to analyze organochlorine were obtained by using higher than room temperature, agitation of the sample, extraction time of 40 min, and polyacrylate fiber.