Capillary electrophoresis (CE) interfaced with low-temperature (4.2 K) fluorescence line-narrowing spectroscopy (FLNS) is used for the separation and spectral characterization of closely related analytes. In this paper, the CE-FLNS system is applied to the analysis of a mixture of deuterated and protonated benzo[a]pyrene, a mixture of structurally similar benzo[a]pyrene and benzo[e]pyrene, and mixtures of dibenzo[a,l]pyrene-derived adenine DNA adducts. The CE-FLNS system provides on-line separation and high-resolution spectroscopic identification of CE-separated analytes, via fingerprint structure of vibrationally resolved FLN spectra at 4.2 K. The combination of the separation power of CE and the spectral selectivity of FLNS provide a methodology that has potential to become a powerful tool for molecular analyte characterization. The main applications of the CE-FLNS system, due to its selectivity, should be in the chemical analysis of structurally similar analytes and applications where analyte purity and detailed structural characterization are required.
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