GC-mass and CG-FTIR spectral data together permit the rapid identification of the histrionicotoxin (HTX) alkaloids. 13C-NMR chemical shifts (δc) are reported for HTX 235A and revised δc are tabulated for nine HTXs and a perhydro-derivative. A butylboronic acid HTX derivative offers GC-MS and GC-FTIR advantages. Artefactural trans diene photoisomers of the HTX class are described as are formaldehyde condensation products. Two new HTX alkaloids 261 and 265E, are characterized by mass and FTIR spectra. © 1992.