The objective of this project is research on and development of new mass spectral techniques in order to provide new and/or more rapid solutions to problems involving (1) chemical structure determination, (2) complex mixture analysis and (3) measurement of trace components in biological systems. The scope and utility of these mass spectral methods are evaluated, and a comparison to other types of analyses, both new and established, is carried out. Fast atom bombardment mass spectrometry and combined liquid chromatography-mass spectrometry are the techniques of current interest. Fast atom bombardment mass spectrometry in both the positive and negative ion mode continues to be applied for the rapid structure confirmation and determination of nucleosides, nucleotides, natural products and synthetic intermediates and products. On-line micro-column liquid chromatography has been combined with a continuous- flow fast atom bombardment ionization interface for the analysis of nucleotides and conjugated metabolites. The use of quaternary amine surfactants to enhance sensitivity in fast atom bombardment mass spectrometry and increase separation and resolution in pairedion reverse phase micro-column liquid chromatography has been evaluated.