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A high-pressure anion-exchange chromatographic system has been modified to provide measurement of large numbers of molecular constituents in serum and for direct comparison to similar measurement in urine. Operating parameters have been adopted which greatly extend the range of elution for strongly retained anionic constituents and limit resolution of early-eluting basic and neutral compounds which were of less interest in this study. Dual monitoring by UV absorption and fluorescence produced by cerate oxidation provides both sensitive and wide-ranging detection capability. Comparative serum and urine chromatograms for a clinically normal subject, a subject after ingesting the drug 4-hydroxyacetanilide, and an infant suffering from extreme acidosis, illustrate the potential usefulness of this analysis in studying the origin, transport, in vivo reactions, and disposition of metabolites.