AbstractThe roots ofMargaretta rosea Oliv., subsp.rosea Bullockcontain cardenolides mixed withKeddenegative ester glycosides. 6 Cardenolides were identified by paper chromatography (PC) and thin layer chromatography (TLC). Three of them were free aglycones (uzarigenin (1), corotoxigenin (3) and coroglaucigenin (5), the other three their corresponding 6‐deoxy‐β‐D‐allo‐pyranosides (ascleposide (2), gofruside (4) and frugoside (6). Only two cardenolides (1and5) were isolated in crystalline form. The behaviour of the more polar portion of the glycoside mixture shows thatD‐gluco derivatives of at least 5 of the 6 cardenolides mentioned were also present.TheKedde.negative glycosides were a complicated mixture containing mainly 2,6‐dideoxysugars linked to esterified polyhydroxy‐pregnanes. After mild acid hydrolysis cymarose, oleandrose and digitoxose could be identified by PC and TLC. From the crude aglycone portion only one cristalline genin (M) could be isolated. This was still a mixture, but its main component according to the mass spectrum was a monobenzoyl derivative C28H38O7. ‐ A small amount of cristalline O‐acetyl‐β‐amyrin was isolated from t