A unique laser-based method was developed for the solid-matrix fluorescence characterization and identification of tetrols, which are the hydrolysis products from benzo[<i>a</i>]pyrene-DNA adducts. By employing different gatewidths with a boxcar integrator, we obtained the fluorescence spectra of the four tetrol isomers adsorbed on 10% α-cyclodextrin/NaCl at several temperatures. The data showed that the fluorescence spectral characteristics of the tetrols were both gatewidth- and temperature-dependent. The experimental conditions were optimized to identify the tetrols which had only minor structural differences. Applications of the gatewidth-dependence method both at room temperature and low temperature were considered. The low-temperature approach has the potential for the application to several species over a range of fluorescence lifetimes. The differences in the fluorescence spectral properties were partially explained by the rotation of functional groups in the tetrols and the solid matrix during the time frame of obtaining the spectra. Comparisons were made among the solid-matrix fluorescence spectra and the solution fluorescence spectra of the tetrols, and the solution fluorescence spectra of pyrene and the solid-matrix fluorescence spectra of pyrene.
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