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Surface plasmon resonance was used to detect oligosaccharides derived from glycoproteins. No sample derivatization or labeling is required for this technique. Sensor surfaces were prepared by immobilizing lectins. In the case ofSambucus nigraagglutinin reactive to terminal sialic acid orRicinus communisagglutinin preferring terminal β-linked galactose, femtomole levels of oligosaccharides could be detected. Using this affinity detector system, oligosaccharides and glycopeptides from a chromatographic separation on a gel filtration column were detected either by on-line monitoring or by analyzing the fractions individually.