Abstract: A new method was proposed for the determination of phenol and hydroquinone in cosmetics by gas chromatography-mass spectrometry. The samples were extracted by methanol, the purified extracts were separated by HPINNOWAX capillary column and detected in the selected ion monitoring (SIM) scanning mode. The results showed that the linear range of phenol was 0.01 ~50 μg/mL(r =0.999 96) and the detection limit was 0.05 μg/g, the recovery rate of sample was 91.3% ~99.6% and the relative standard deviation was 1.5% ~6.0%. The linear range of hydroquinone was 0.02 ~50 μg/mL (r= 0.999 87) and the detection limit was 0.10 μg/g, the recovery rate of sample was 91.5% ~ 99.7% and the relative standard deviation was 3.2% ~ 5.4%. The method is simple, rapid and sensitive, and can effectively eliminate the interference of cosmetic matrix. It is suitable for the qualitative and quantitative determination of phenol and hydroquinone in cosmetics.