Abstract: High performance liquid chromatography (HPLC) and nuclear magnetic resonance spectrometry (NMR) were applied to the identification and determination of alkylphenol ethoxylate (APEO) in textiles and auxiliaries. Retention time of chromatograph and 1HNMR was used in the qualitative analysis of APEO,and the method of external standard calibration of HPLC was used for its quantitative determination. In the HPLC determination,a mixed solution of methanol and 0.01 mol·L-1 ammonium acetate solution was used as mobile phase,and UV-detection at 277 nm was selected. Linear relationship between the peak area and concentration of APEO was obtained in the range of 5-250 mg·L-1 (r=0.992 8),with a detection limit of 1.0 mg·kg-1. Values of RSD′s (n=5) in measurements of retention time were less than 0.21%,and in measurements of peak area were less than 3.69%. Results of recovery test obtained were in the range of 91%-98%. The proposed method has been applied in the entry-exit inspection of textile and auxiliaries satisfactorily.