Abstract: Aroma characteristics of Guipu No.3 grape skin residue spirits were investigated in this research. Different proportion of water and sugar were added in Guipu No.3 grape skin residue. Spirits were obtained through fermentation and distillation. Volatile components of distilled spirits samples were analyzed by the headspace-solid phase microextraction method combined with gas chromatography-mass spectrometry (GC-MS). Method of odor activity values (OAV)was applied to identified the active and characteristic volatiles, in order to distinguish aroma characteristics in spirits of different ratio water added. Results showed that Guipu No.3 skin residue spirits provided high aroma quality. Characteristic volatiles including ethyl hexanoate, isoamyl acetate, ethyl crotonate, damascenone, ethyl butyrate, ethyl acetate, ethyl caprylate, ethyl caprate were identified, contributing aroma notes of fruit, sweet, flower and bouguet to Guipu No.3 spirits. According to results of volatiles content and characteristic aroma components, a conclusion was drawn that spirits made from skin residue with two double water added could gain best aroma quality.