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In this chapter, we describe a method to identify amino acids (AA) by capillary electrophoresis in conjunction with light-emittingdiode-induced fluorescence (LEDIF). First, amino acids labeled with naphthalene-2,3-dicarboxaldehyde (NDA) in the presenceof cyanide are converted to highly fluorescent cyanobenz[
f
]isoindole (CBI) derivatives. Next, they are separated by gel electrophoresis in the presence of EOF. In the process, theCBI products were excited by a violet LED to produce green fluorescence. In addition to the optical setup of light-emittingdiode-induced fluorescence, the preparation of poly(ethylene) oxide for amino acid separation is also described in this chapter.