In order to determine the composition and content of eluent wastewater from the production of nitroglycerin/1，2，4-butanetriol trinitrate （NG/BTTN） mixed nitrate， a high performance liquid chromatographic （HPLC） gradient elution method was carried out to detect washing wastewater. The chromatographic conditions were determined as follows： the stationary phase was C18 （250 mm×4.6 mm， 5 μm） column， the mobile phase was acetonitrile/water solution， and and the detection wavelength was 200 nm. The results showed that six organic compounds were detected in the scrubber wastewater. By fitting the retention time of the compounds and their linear relationship with the partition coefficient LogD （27 samples were taken within 7 days）， it was determined that in addition to NG and BTTN， the following compounds were present in the scrubber wastewater from the production of mixed NG/BTTN nitrates： 1，2-dinitroglycerol（30.58%-41.20%）， 1，3-dinitroglycerol（110.69%-135.14%）， 1，2，4-butanetriol-1，2-dinitrate（7.90%-10.63%）， and 1，2，4-butanetriol-1，4-dinitrate（22.55%-27.95%）， with the standard deviations lower than 10%， and the method was sampled for 40 times within 10 d. It was proved that the method is accurate， reliable and applicable， and meets the testing needs of industrial production.