The determination of polyalcohols in vinegar by GC-MS was developed.The vinegar sample was extracted by acetonitrile and the oximation was introduced for reducing matrix interference,which was derived by glucose condensation while the acetylation was going with acetic anhydrid.The limit of the method was 0.020mg/L,the recoveries was between 93% and 105%,with RSD between 2.8% and 10.5%.The test result showed: the content of erythritol in Shanxi extra aged vinegar was more than others,and there was few polyalcohols detected in alcohol vinegar.The determination of polyalcohols should help identify geographical indication vinegars.