Abstract: In this paper, the organic substances in drinking water were analyzed by GC-MS (Gas Chromatography/Mass Spectrometry). The sample was selected in two ways, one was from the tap water, and the other was from ground water. The samples were passed through the column, which was filled with XAD-2 absorbed resin and the column was rinsed by methane dichloro. The rinsed solution was concentrated by N 2. Nine compounds from tap water and ten ones from well water were separated and identified according to their mass spectra. The results showed that simple sample pretreatment and high recovery were proved.