Cardiac glycosides from Yellow Oleander (Thevetia peruviana) seeds

► Seeds of Thevetia peruviana contain a mixture of at least six glycosides. ► The structures of two unknown thevetia glycosides were determined. ► Preparative HPLC made the glycosides available in their pure form. ► Aglycone preparation required acid cleavage of the sugars under severe conditions. ► The analytical techniques comprised LC-MS(/MS), (high-resolution) GC-MS, and NMR.