In this study acrylamide was determined with the aid of single drop microextraction and gas chromatography, by means of electron capture detector (ECD).Influence of experimental parameters such as extraction solvent, salt effect, extraction time and temperature on the extraction yield examined and the extraction carried out in the optimized conditions of octanol solvent including 33% (w/v) sodium chloride in 5 (min) at room temperature. Prior to extraction, the derivatization process of acrylamide was done by adding of hydrobromic acid and ammonium peroxydisulphate under the conditions of 45 ? c, in 15 min. finally 1 µL of extractive sample was injected to the gas chromatography with ECD. Limit of detection and RSD and dynamic range of this procedure for existing acrylamide in water samples were estimated 0.6 µgl -1 and below 6 % and 1-100 µgl -1 , respectively; eventually the method was employed for real sample analysis of bread, potato chips and cake.