A rapid method for the simultaneous determination of polyoxyethylene octylphenol ether（OPEO） and polyoxyethylene nonylphenyl ether（NPEO） was developed by using high performance liquid chromatography-mass spectrometry（HPLC-MS）.The samples were ultrasonically extracted with methanol.Chromatographic analysis was carried out on an Agilent Eclipse Plus C18（4.6 mm×100 mm,3.5 μm） column with 5 mmol/L ammonium acetate solution-methanol as mobile phase in gradient program,and the quantitation was performed by the matrix-matched external standard method.The standard addition recovery experiments were conducted on two different kinds of wall coating（A and B）.The calibration curves showed good linearities in the concontration range of 0.1-5.0 mg/L with correlation coefficients greater than 0.99.The recoveries of alkylphenol ethoxylates at three spiked levels ranged from 83.8% to 114.5%,with relative standard deviations（RSDs,n=6） of 1.3%-9.8%.The quantitation limits were between 4.0 mg/kg and 5.5 mg/kg.The method is simple,time-saving and environmental friendly with high sensitivity and good reproducibility,and has a practical application value due to its low-cost and short-circle.