The aim of this study is to use a very small amount of extraction solvents and select the low toxicity extraction solvents with simple preconcentration processing of rapid extraction of nitrophenolic compounds in water samples, in order to comply with environmental protection and achieve the goal of analytic efficiency.In this study, we use ultrasound-assisted emulsification microextraction (USAEME) method based on solidification of floating organic drop combined with ultra performance liquid chromatography (UPLC) to determine nitrophenols in aqueous sample.Choose low toxic extraction solvent (1-undecanol) and use hand-assisted ultrasound method to disperse it without using any dispersive solvents; meanwhile, greatly reduce the amount of extraction solvents we used (Extraction solvent: 12μL).The detection limits of the method ranged from 1.4 to 6.4μg L-1 for spiked lake water and 1.5 to 6.9μg L-1 for spiked field water.The precision of the method ranged from 5% to 11%.