Abstract: A method for determination of 3 phenol phosphates i.e., tricresyl phosphate (TCP), cresyl diphenyl phosphate (CDP) and trixylenyl phosphate (TXP), in nipple by GC-MS was proposed. The 3 phenol phosphates in sample was extracted with ethyl acetate, and the extracts were concentrated by rotary evaporator in a water bath at 35 ℃. The residue obtained was dissolved and made up to 2.0 mL with methanol, which was used for GC-MS analysis. The DB-1701 capillary chromatographic column (30 m×0.25 mm, 0.15 μm) was used for separation, and the electron impact ionization source with selected ion monitoring (SIM) was adopted in MS. Linear relationships were obtained between values of peak area and mass concentration of the 3 phenol phosphates in the same range of 30.0-500 μg·L-1, with lower limit of determination (10S/N) of 30 μg·kg-1. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery and RSD′s (n=10) found were in the ranges from 64.0% to 88.5% and 0.86% to 8.7% respectively.