Establish a solid phase extraction-high performance liquid chromatography(HPLC)analysis method with double detector to simultaneously determine atrazine and benzopyrene in water.Methods Atrazine and benzopyrene. In was enriched by large volume solid-phase extraction column and eluted by methylene chloride. Gradient elution was performed on Eclipe XDB-C₁₈ (150 mm×4.6 mm, 5 μm) analytical column with acetonitrile-water as mobile phase. The products were then determined by diode array detector (DAD) and fluorescence detector (FLD). Results The linear range of the method of atrazine and benzopyrene was 50-800 μg/L and 5.19-83.04 μg/L, respectively. The correlation coefficients (r) were both over 0.999. The limits of detection were 0.01 and 0.000 5 μg/L, the limits of quantification were 0.03 and 0.001 5 μg/L, and the average recoveries of atrazine and benzopyrene in water were 88.9% and 90.4%, respectively. The relative standard deviation was less than 6.8%.Conclusion This method was accurate, sensitive and applicable for determining atrazine and benzopyrenein water samples.