Chromatographic procedures (HPLC, GC-MS) are outlined in this paper for the analysis of alkaloids in poisonousDatura ferox seeds of Argentina, from which previously only quantitative analysis for scopolamine was known. Five additional tropane alkaloids are now identified as 3α-tigloyloxytropane (tigloyltropeine), 3-phenylacetoxy-6β,7β-epoxytropane (3-phenylacetoxyscopine), aposcopolamine (apohyoscine), 7β-hydroxy-6β-propenyloxy-3α-tropoyloxytropane, traces of 7β-hydroxy-6β-isovaleroyloxy-3α-tigloyloxytropane and a pyrrolidine alkaloid, hygrine. Two new structures, 3-phenylacetoxy-6β,7β-epoxytropane (3-phenylacetoxyscopine) and 7β-hydroxy-6β-propenyloxy-3α-tropoyloxytropane, are proposed on the basis of their spectra. Hyoscyamine, nicotine and tropane N-oxides were not detected in all samples studied.