Abstract: The method of GC-MS combined with liquid-liquid extraction was used for the determinaiton of on of 24 semi-volatile organic compounds (SVOCs) in environmental water. The sample was extracted with dichloromethane. The extracted solution was concentrated and re-dissolved and then separated on a DB-5MS capillary column. EI-SIM was adopted in MS. The linear relationship was found between the peak area and the mass concentration of the 24 SVOCs was in a certain range,with detection limits in the range of 0.03-0.28 μg·L-1. The recovery rates measured by standard addition method were in the range of 70.1%-128%,with RSD was less than 6%. The actual sample analysis results showed that those SVOCs such as the nitrochlorobenzenes,chlorophenols and phthalate esters were detected in the water samples of surface water and chemical wastewater somewhere.