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A new cycloartane triterpenoid, 24-acetylcyclocantogenin (1), along with five cycloartane triterpenoids (2-6), eight steroids (7-14) and nine other known compounds (15-23), was obtained from the methanol extract of roots of Astragalus polycladus var. nigrescens. Their structures were elucidated based on extensive spectroscopic analysis (1D and 2D-NMR, MS and IR). They were isolated from A. polycladus var. nigrescens for the first time.