Abstract: In order to improve the signal strength and the degree of separation in GC-MS, Jasminum Sambac Ait was separated by molecular distillation. Jasminum Sambac Ait was separated into three segments (under 60℃, 60⁹0℃, over 90℃) by molecular distillation, according to each segments' characteristic, the conditions of Molecular Distillation and GC- MS were optimized. It was found that the resolution and intensity of components in chromatographic peaks were enhanced, the same as similarity. Fifty-nine compounds were identified, thirty-five of which were the first reported. Results showed that the method could reflect the material composition more completely, because of the advantages of the molecular distillation in separation of flavors and fragrances with heat-sensitive and easily oxidized. The analysis result could provide guidance for the blend and product development of flavors and fragrances.