We have investigated two species of Senecio from the flora of Azerbaidzhan: S. rhombifolius (Willd) Sch. Bip. and the endemic, previously unstudied S. kubensis Grossh. For S. rhombifolius, using a published method, we isolated 1.34% of combined alkaloids (76.87% N-oxides) from the epigeal part and 3.68% (97.88% N-oxides) from the subterranean part, and identified platiphylline (I), seneciphylline (II), and neoplatiphylline (III) via comparisons of Rf values, IR/UV spectra, and melting points with authentic samples. For S. kubensis, collected in the flowering phase, the epigeal part yielded 0.45% combined alkaloids (67.86% N-oxides) and the subterranean part 0.51% (40% N-oxides); seneciphylline was isolated from both parts, accounting for 89.32% (epigeal) and 75.21% (subterranean) of the total alkaloids, identified by direct comparison with an authentic sample.