The dissolved organic matter (DOM) of acrylonitrile-butadiene-styrene (ABS) resin wastewater was qualitatively analysed by gas chromatography with mass spectrometry(GC-MS), Fourier transform infrared spectrometer(FTIR) and three-dimensional excitation–emission matrix (EEM) fluorescence spectroscopy. The detected results shows that the GC-MS qualitatively analysed 21 dissolved organic pollutants, such as acetophenone, styrene, alpha, alpha-dimethyl-benzenemethanol, 3,3′-oxybis-propanenitrile, 3,3′-iminobis-propanenitrile, 3,3′-thiobis-propanenitrile, 3-(dimethylamino)-propanenitrile and 2-propenenitrile. The results of Fourier transform infrared spectrometer (FTIR) and three-dimensional excitation-emission matrix (EEM) fluorescence spectroscopy could examine and certify the accuracy and integrity for the qualitative analysis of GC-MS. The results of this study provides an important guiding role for the development of wastewater treatment process.