In this study, a gas chromatography-mass spectrometry (GC/MS) method was established for the determination of geranyl nitrile, 2-pentyl-2-cyclopenten-1-one and phenyl cyanide in fragrance compound, and the method was also validated. The method had good linearity (>0.990 0) with the concentration from 0.000 5 mg/mL to 0.100 0 mg/mL and low limits of detection (LOD) (<0.005 μg/mL) for these three target compounds. And the recovery was from 90% to 116% with relative standard deviation (RSD) from 4.2% to 5.4% at quality control concentration. In a word, the method met the need of trace detection, which can be used to test geranyl nitrile, 2-pentyl-2-cyclopenten-1-one and phenyl cyanide in fragrance compound. When the GC-MS method was applied to detect these three components in different pepppermint fragrance samples, none of them was detected out.