Presented is a fluorometric technique for the quantitative analysis of taurine in biological samples. The sample is homogenized, treated with picric acid, and passed through a mixed-bed, ion-exchange column. The eluant is lyophilized, reconstituted, and an aliquot derivatized with o-phthalaldehyde (OPA) prior to high performance liquid chromatography (HPLC). The ion-exchange column removes all amino acids, cysteic acid, phosphoethanolamine, and hypotaurine while allowing quantitative recovery of taurine. Using the procedure as outlined, quantitation has been performed from 0.080-1.6 nmoles per analysis. The lower limit of quantitation, using the equipment specified, was shown to be 5 pmoles per analysis. The method allows rapid sample processing while maintaining a high degree of sensitivity and accuracy.