A rapid and environmental-friendly analytic method was established for the determination of deoxynivalenol(DON)in grain samples.The samples were extracted with water, cleaned up with immunoaffinity column（IAC）.The separation of targeted compound was performed on a Waters Acquity UPLC BEH C18（2.1 mm×50 mm, 1.7 μm） using methanol-water（10∶90） as mobile phase with a flow rate of 0.1 mL/min at 25 ℃.The injection volume was 1 μL for UV detection at 220 nm and the retention volume was less than 0.5 mL.The whole process from sample pretreatment to analysis took less than 45 min.The linear range of deoxynivalenol was in the range of 0.5 -10.0 mg/L with a correlation coefficient of 0.999 96.The limit of detection（LOD） was 0.15 ng and the limit of quantitation（LOQ） was 0.5 ng.The average recoveries were between 84% and 98% with RSDs of 2.9%- 5.9%.The method was suitable for the determination of DON in the raw grain, with advantages of simplicity, rapidness, sensitivity, good reproducibility and environment friendly.