Monosaccharide composition of glycans based on Q-HSQC NMR

•A method to determine the monosaccharide composition based on NMR was developed.•Q-HSQC depends of a JCH value of 155Hz for C-1, allowing milli-microM detection.•Analysis of the native and hydrolyzed glycan give insights of the molecular mobility. Glycans have essential functions related to structu...

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Veröffentlicht in:Carbohydrate polymers 2014-04, Vol.104, p.34-41
Hauptverfasser: Sassaki, Guilherme Lanzi, Guerrini, Marco, Serrato, Rodrigo Vassoler, Santana Filho, Arquimedes Paixão, Carlotto, Juliane, Simas-Tosin, Fernanda, Cipriani, Thales Ricardo, Iacomini, Marcello, Torri, Giangiacomo, Gorin, Philip Albert James
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container_start_page 34
container_title Carbohydrate polymers
container_volume 104
creator Sassaki, Guilherme Lanzi
Guerrini, Marco
Serrato, Rodrigo Vassoler
Santana Filho, Arquimedes Paixão
Carlotto, Juliane
Simas-Tosin, Fernanda
Cipriani, Thales Ricardo
Iacomini, Marcello
Torri, Giangiacomo
Gorin, Philip Albert James
description •A method to determine the monosaccharide composition based on NMR was developed.•Q-HSQC depends of a JCH value of 155Hz for C-1, allowing milli-microM detection.•Analysis of the native and hydrolyzed glycan give insights of the molecular mobility. Glycans have essential functions related to structural architecture and specific cell surface phenomena, such as differentiation, biosignalling, recognition and cell–cell interaction, with the carbohydrate structure determining main function in the cell. Due to the importance of the primary structure, the monosaccharide composition is crucial to show the glycan structure. We now present a method for complex carbohydrates based on NMR spectroscopy, which has shown to give similar results to those obtained by the classic GC–MS-carboxy-reduction/deuterium labeling approach. Quantitative HSQC, through JCH dependence showed 155Hz as the best value for 1H/13C anomeric aldoses, allowing milli-microM detection using conventional inverse probe heads. Combining the quantification of native monosaccharide units of the glycan and those from the hydrolyzed product, a strong correlation occurs between the molecular mobility of the monosaccharide units, giving rise to some insights on the dynamic properties of the parent glycan.
doi_str_mv 10.1016/j.carbpol.2013.12.046
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subjects Applied sciences
Carbohydrate quantification
Dynamics
Exact sciences and technology
Glycoconjugates
Magnetic Resonance Spectroscopy - methods
Monosaccharides - analysis
Mutarotation
Natural polymers
Physicochemistry of polymers
Polysaccharides
Polysaccharides - chemistry
Starch and polysaccharides
title Monosaccharide composition of glycans based on Q-HSQC NMR
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