A new method for the determination of hydroquinone and phenol in freckl-removing cosmetics by Gas Chromatography/ Mass Spectrometry/ Single Ion Monitor Method was developed.The hydroquinone and phenol in samples were extracted by ethanol with supersonic wave. The m/z110 and m/z94 were monitoring ion of hydroquinone and phenol, respectively. The method was simple,rapid and accurate. The detection limit of hydroquinone and phenol were 0.1 ng and 0.05 ng, respectively. The recovery were 91.5%~102% for hydroquinone and 86.5%~98.7% for phenol with the RSD of 1 41% and 0 41%.