A technique for resolving amino acid enantiomers on a 12-ft packed column has been adapted to the analysis of fossils and other materials. The synthesis of the resolving agent, N-trifluoroacetyl-L-prolyl chloride, along with preparation of solid support and other necessaryreagents, is described. Representative chromatograms are presented, as well as data on the accuracy and precision of the technique. -- AATA