A new method to determine benzene and toluene contents in water samples was established by the combination of dispersive liquid-liquid microextraction(DLLME) and gas chromatography. The capillary column was used for the separation, the hydrogen flame ionization detector(FID) was use to analyze the samples by using CHCl3 as extractant, acetone as dispersant. The method has been successfully used to detect benzene substances in different water quality.