Abstract: The surface water, industrial wastewater, or seawater samples was rapidly collected by filling the sample bottles completely, and the internal standard fluorobenzene was added online. Both the samples and internal standard were simultaneously subjected to purge-and-trap analysis under the conditions of purge time of 10 min, purge temperature of 40 °C, desorption temperature of 180 °C, and desorption time of 2 min, and then 1,3-butadiene and 1-bromopropane were determined by gas chromatography-mass spectrometry. In the chromatographic analysis, separation was performed on DB-624 column as the stationary phase under temperature-programmed mode. In the mass spectrometric analysis, ionization was conducted by electron impact ion source, and detection was made in the selected ion monitoring mode. It was shown that linear ranges of 1,3-butadiene and 1-bromopropane were found in the range of 1.0-40.0 µg · L⁻¹, with detection limits (3.143s) of 0.3, 0.2 µg · L⁻¹, respectively. Spike recovery tests were made on the 3 aforementioned sample matrices at 3 concentration levels, giving recoveries in the range of 81.4%-118%, and RSDs (n=6) of the determined values ranged from 1.7% to 12%.