Herbicide wastewater is one of tne industrial wastewater, it has high salt content, poor biodegradability, biodegradable characteristics. Nitrogen-containing organic compounds are dominated in dissolved organic matter and dissolved organic matter of wastewater, BOD: COD = 0.045, C:N:P = 692:426:1. Applying static headspace, purg and trap, solid-phase extraction, solid-phase microextraction and liquid-liquid extraction as pretreatment methods combined with gas chromatography/mass spectrometry (GC/MS), which qualitatively analyzed the organic components of the Atrazine, acetochlor herbicide production wastewater and researched the UV spectrum, three-dimensional fluorescence spectroscopy of the wastewater and its major pollutants. The study of GC/MS indicated that Wastewater contained chlorinated hydrocarbons, BTEX and triazines, amides herbicides etc. 38 kinds of volatile and semi-volatile organic compounds, atrazine and acetochlor herbicides accounted for 87. 99%. Affected monocyclic or heterocyclic substances, the ultraviolet absorption spectrum of the wastewater in 210-230 and 250-270 nm in that the amino group lead to the UV absorption red shift 20 nm. Wastewater generated 5 fluorescence peak in λ(ex)/λ(em) = 200-280/300-400 nm, such as a(225/305 nm), b(265/365 nm), c(275/305 nm), d(285/390 nm), e(320/375 nm). Based on three-dimensional fluorescence results of the different functional groups of the characteristics organic, fluorescent area of unsaturated bond is in λ(ex)/λ(em) = 215-230/290-340 nm, the main contribution of the fluorescent substance in the region were olefins, benzene, heterocyclic in the wastewater; fluorescent area of Phenolic hydroxyl and carbonyl is in λ(ex)/λ(em) = 270/300 nm, the main contribution of the fluorescent substance in the region were phenols, ketones.