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The purification of oligosaccharides and glycopeptides presents many problems, not the least of which is the diversity of possible structures. To date no single chromatographic or electrophoretic method has been proven to separate all oligosaccharide isomers in a buffer system that is compatible with immediate nuclear magnetic resonance spectroscopy (
NMR
) or mass spectrometry (MS) analysis. In addition, the inherent nonchromogenic nature of oligosaccharides often makes their on-line sensitive detection very difficult. This chapter details the range of high-resolution chromatographic techniques available to glycobiologists either utilized singly or in concert to achieve the separation of pure oligosacccharides. Included are methods for the release of oligosaccharides and monosaccharides from glycoprotems, as well as methods for then separation and sensitive detection.