The mass spectral fragmentations of 2-oxosparteine (lupanine), 2-oxo-a-isosparteine (a-isolupanine), 15-oxosparteine, 17-oxosparteine and 10-oxosparteine (aphylline) are reinvestigated and discussed. Fragmentation pathways, elucidation of which were assisted by accurate mass measurements and metastable transitions, are proposed. The fragmentation assignments are not consistent with those previously reported in the literature. Many fragment species of the same m/z (low-resolution spectra) are composed of two or three fragment ions of Merent elemental compositions (high-resolution spectra). The obtained data create a safe basis for distinguishing structural and stereo isomers.

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Two‐dimensional phase‐sensitive homo‐ and hetero‐nuclear shift correlation methods, in addition to homo‐ and hetero‐nuclear relayed coherence transfer, COLOC and NOESY experiments, were used to obtain a complete proton and 13C assignment of α‐isosparteine methiodide and α‐isosparteine methylene diiodide.