A new protocol for the extraction and analysis of intracrystalline mac
romolecules has been developed that allows the rapid determination of
the amino-acid composition of fossils. The technique utilizes decalcif
ication with 2 M HCl, characterization of the soluble fraction of the
biomolecules by automated amino-acid analysis, and differentiation usi
ng multivariate statistics. Compared to other methods, this technique
allows sampling of indigenous degraded proteins in addition to the pre
served remains of peptides, leading to the recovery of data from more
reliable indigenous sources. Although the extraction method is demonst
rated using fossil samples to demonstrate gross phylogenetic differenc
es, there is much potential to use these biomolecules for a wide range
of applications.