In this investigation, solid phase extraction (SPME) is applied in order to determine the concentrations of insecticides and rat poisons detected in the samples taken on the industrial finished product. Gas chromatography, coupled with mass spectroscopy (GC-MS) is used as an analytical instrument for this purpose. In order to obtain an optimal extraction, different process parameters are examined and optimized. Relevant results are obtained using 30 minutes non-specific binding property time, with 30 minutes stirring mode with magnetic stirring and a temperature of 30 °C. The efficiency of insecticides, poisons for rats, has been demonstrated and pesticides are likely to be at a high concentration in finished industrial products.