Abstract: A method of HPLC-MS for determination of octylphenol (OP) and octylphenol polyoxyethylene ether (OPOE) in textile was proposed. The OP and OPOE in textile were extracted with methanol; the extract obtained was evaporated and made up to 10 mL with methanol. C18 reversed phase column was used as stationary phase and a mixture of methanol and water (80+20) was used as mobile phase. ESI was adopted in MS. Linear relationships between values of peak area and mass concentration of OP and OPOE were kept in the same range of 0.01-0.5 mg·L-1, with values of lower limit of determination (10S/N) of 0.07 and 0.05 mg·kg-1 respectively. Tests for recovery were made at the concentration levels of 0.5, 1.0 and 2.0 mg·kg-1 of the mixed standards, values of recovery found were in the ranges of 90.5%-108% for OP and 91.4%-109% for OPOE with RSD′s (n=7) less than 8%.