Nine cardenolide glycosides and one aglycone, including five new compo
unds, were isolated from the aerial parts of the milkweed, Gomphocarpu
s sinaicus. The elucidation of the structures and stereochemistry of t
he new glycosides was accomplished using FAB mass spectrometry, H-1 NM
R, C-13 NMR, H-1-H-1 COSY, H-1-C-13 COSY, NOE and NOESY. The new compo
unds were identified as 7,8-dehydrocalotropin, 17 alpha-hydroxy-7,8-de
hydrocalotropin, 19-acetylglucocoroglaucigenin, 19-acetylglucofrugosid
e and humistratagenin. Some of these results differ from those reporte
d in three recent publications on the cardenolides of the same plant s
pecies.