Abstract: The method of HPLC-MS was applied for determination of alkylphenol ethoxylates in household paper. The sample was shredded and extracted with acetonitrile by ultrasonic. The extract was separated on Dikma Inspire HILIC column using the mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution as mobile phase for gradient elution. ESI+ and SIM were adopted in MS. Linear relationship was found between the peak area and the mass concentration of alkylphenol ethoxylates with different degree of polymerization in a certain range, with limits of quantification (10S/N) in the range of 1.0-4.3 μg·kg-1. Recovery rates measured by standard addition method were in the range of 51.0%-117%. The method was applied to analyze alkylphenol ethoxylates in household paper, giving values of RSD (n=6) in the range of 2.4%-12%.