A new polyacetylene compound (4), (6E, 12E)-tetradecadiene-8, 10-diyne-1, 3-diol diacetate has been isolated along with (4E, 6E, 12E)-tetradecatriene-8, 10-diyne-1, 3-diol diacetate and atractylenolide I from Atractylodes Rhizome. The structure of 4 was determined on the basis of its spectral data and chemical reaction.