Abstract:A method for the determination of 29 semi-volatile organic compounds in drinking water by large volume injection-gas chromatography-mass spectrometry was established. The samples were extracted by liquid-liquid extraction with methyl tert-butylether solvent, and the samples were injected in large volume by solvent emptying mode programmed heating up. Multi-Reaction ion Monitoring (MRM) and internal standard method were used to quantify the samples. Results: The calibration curves were linear in the concentration of 0.2~10.0 μg/L, and the correlation coefficient was greater than 0.994. The detection limits of the method was in the range of 0.003~0.110 μg/L, the recovery rates was in the range of 61.7%~108.6%, and the relative standard deviation was in the range of 1.5%~8.7%. The method is simple, sensitive and accurate, which is suitable for the detection of 29 semi-volatile organic compounds in drinking water.