A procedure is described for the determination of aminated monosaccharides at nanomolar concentrations by derivatization with the fluorogenic reagent 3-(p-carboxybenzoyl)quinoline-2-carboxyaldehyde (CBQCA) to produce a fluorescent derivative that can be identified and detected by capillary electrophoresis with laser-induced fluorescence detection. Labeling conditions that favor the formation of the CBQCA-aminated sugar derivative over secondary fluorescent products were chosen. Samples as dilute as 1.0 × 10-9 M 1-gluocosamine were analyzed. The results can be extended to other aminated monosaccharides since they showed similar reaction yields on labeling. The capability for the analysis of mixtures of aminated sugars was also demonstrated. Five labeled aminated sugars were separated by capillary electrophoresis using a running buffer containing a mixture of phenyl boronate and borate. The detection scheme was based on a low-scattering sheath flow cuvette as a postcolumn detector and two photomultiplier tubes that have mutually excluded wavelength ranges to prevent the water Raman band from contributing to the background signal. The system had a limit of detection of 75 zeptomol of fluorescently labeled 1-glucosamine.