Quantitative Verfolgung der Festphasensynthese des Sialyl-Lewis-X-Tetrasaccharids durch Gated-decoupling-13C-NMR-Spektroskopie nach13C-Anreicherung

Advances in the techniques for oligosaccharide synthesis have lagged behind those for other classes of biological oligomers. For the preparation of oligopeptides and oligo- Figure 4. Autoradiograms showing the binding of hybrid 5 to 32 P-labeled DNAs. Lanes 1 ± 6: T/CRE hs , 5: 0, 7.7, 19, 38, 58, 77 nm respectively; Lanes 7 ± 11: T/CRE hs m, 5: 7.7, 19, 38, 58, 77 nm respectively; lanes 12 ± 14: CRE hs , 5: 38, 77, 154 nm respectively. Binding reactions were performed over 10 min at 4 8C using < 1 nm labeled DNAs in a binding mixture (20 mL) containing 20 mm tris(hydroxymethyl)aminomethane (pH 7.5), 100 mm KCl, 2 mm MgCl 2 , 2 mm ethylenediaminetetraacetate, 10 % glycerol, 0.3 mg mL À1 N,O-bovine serum albumin (BSA), and 2 % NP-40. The products were resolved by polyacrylamide gel electrophoresis using a 10 % nondenaturing acrylamide gel and 0.5X TBE (25 mm tris borate and 0.5 mm EDTA) buffer. CRE hs : 5'-d(CGACGTCATCGGAGGTCCT)-3' 3'-d(GCTGCAGTAGCCTCCAGGA)-5'

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Development of an Easy-to-Use Mass Spectrometric Technique to Monitor Solid-Phase Reactions on Polystyrene Supports

Heinze

Winterhalter

Jannack

2000

Chem. Eur. J.

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By using mass spectrometry as an analytical tool to characterise substituted, cross-linked polystyrene resins, it is possible to directly monitor the progress of the solid-phase reactions performed on these resins without prior cleavage of the resin-bound molecules. Therefore, this is a true on-resin analytical method. The mass-to-charge ratios observed in the mass spectra are readily assigned to fragments of the polymer that include the chemically bound substituents. This is the first time that the formation and breaking of bonds have been directly observed on the polymeric support. Furthermore, the relative intensities of the signals in the mass spectra provide a measure of the completeness of the reaction. Because these measurements are rapidly performed without further chemical transformations or cleavage procedures, and because only minimal amounts of material are needed, this technique could become the solid-phase equivalent of thin-layer chromatography used in classical liquid-phase chemistry.

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Quantitative Verfolgung der Festphasensynthese des Sialyl-Lewis-X-Tetrasaccharids durch Gated-decoupling-13C-NMR-Spektroskopie nach13C-Anreicherung

Cited by 9 publications

References 21 publications

Fluorinated Protective Groups for On-Resin Quantification of Solid-Phase Oligosaccharide Synthesis with19F NMR Spectroscopy

Fluorinated Protective Groups for On-Resin Quantification of Solid-Phase Oligosaccharide Synthesis with19F NMR Spectroscopy

Solid-Phase Capture-Release Strategy Applied to Oligosaccharide Synthesis on a Soluble Polymer Support

Development of an Easy-to-Use Mass Spectrometric Technique to Monitor Solid-Phase Reactions on Polystyrene Supports

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