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Iii order to simplify a laser fluorometric detector for capillary electrophoresis, a semiconductor laser emitting at 660 nm is used as an exciting source. A labeling reagent fluorescent in the deep-red region is newly synthesized and used for determination of amino acids. The separation resolution is several hundred thousand and the detection limit is subattomole levels. Protein is also labeled by the dye developed and is measured at subfemtomole levels. Contrarily, nonfluorescent samples are detected by indirect fluorometry. Amino acids, flavin adenine dinucleotide (FAD) and deoxyadenosine monophosphate (dAMP) are determiiied, the detection limit being subpicomole levels.