Abstract: Blackened jujube wine with alcohol content of 7%vol was used as the base liquor to study the change rules of alcohol content and volatile flavor substances in the distillation process, and the content of volatile substances and sensory evaluation were taken as the criteria to optimize the distillation process of blackened jujube wine. Headspace solid phase microextraction and mass spectrometry were used to detect volatile substances such as esters, alcohols, aldehydes and acids in distilled liquor. The results showed that the alcohol content gradually decreases with the distillation process, and stopped distillation when the alcoholicity was 2.4%vol. In the second distillation process, the contents of alcohol, ester and aldehyde liquor heads were relatively high, and the contents gradually decreased with the distillation process. In some alcohol, acid and aldehyde liquor tails, the contents were relatively high, and the contents increased with the distillation process. Based on two different alcohol distillation and quadratic distillation device as well as wine head to feints the distillate obtained volatile flavor matter contents and sensory evaluation results analysis, the distillation process of blackened jujube wine was finally determined as follows:The volume of the distillate collected from one distillation was 35% of the original solution, the average alcohol contents was 27.4%vol, and the second distillation was intercepted. The volume of liquor head was 2% of the volume of primary distillate, the volume of liquor tail removal was 20% of that of primary distillate, and the volume of total distillate collection was 46% of that of primary distillate.