<jats:title>Abstract</jats:title><jats:p>Three new alkaloids, longistylumphyllines A–C (1–3), together with the six known alkaloids deoxycalyciphylline B, deoxyisocalyciphylline B, methyl homosecodaphniphyllate, daphnicyclidin A, daphnicyclidin B, and daphnicyclidin F, were isolated from the stems and leaves of <jats:italic>Daphniphyllum longistylum.</jats:italic> Their structures and relative configuration were elucidated on the basis of spectroscopic data, especially 1D and 2D NMR techniques.