The capabilities of full fluorescence spectral detection for the analysis of polyaromatic hydrocarbons after a liquid chromatographic separation were evaluated. The limits of detection and the linear dynamic range were determined for three test compounds, benzo[a]pyrene, perylene and anthracene. With the instrument used, detection limits in the micromolar concentration range (ca. 100 ng injected), and a linear dynamic range of at least three orders of magnitude were observed. In addition, the pair of isomers 1- and 2-aminoanthracene, which are incompletely resolved both spectroscopically and chromatographically, were studied. Finally, a commercially available mixture of polyaromatic hydrocarbons was characterized, and it was possible to resolve the chromatographically unresolved pair of isomers benzo[a]anthracene and chrysene. The data analysis methods used included Kalman filter-based methods for adaptive subtraction of background responses, shift correction and linear regression analysis of overlapped responses. The results indicate that full fluorescence spectral detection in liquid chromatography should be an increasingly useful technique.