title: Determination of glucan phosphorylation using heteronuclear 1H, 13C double and 1H, 13C, 31P triple-resonance NMR spectra.
abstract: Phosphorylation and dephosphorylation of starch and glycogen are important for their physicochemical properties and also their physiological functions. It is therefore desirable to reliably determine the phosphorylation sites. Heteronuclear multidimensional NMR-spectroscopy is in principle a straightforward analytical approach even for complex carbohydrate molecules. With heterogeneous samples from natural sources, however, the task becomes more difficult because a full assignment of the resonances of the carbohydrates is impossible to obtain. Here, we show that the combination of heteronuclear (1) H,(13) C and (1) H,(13) C,(31) P techniques and information derived from spectra of a set of reference compounds can lead to an unambiguous determination of the phosphorylation sites even in heterogeneous samples.
authors.affiliation: Leibniz-Institut für Molekulare Pharmakologie (FMP), Robert-Rössle-Str. 10, D-13125, Berlin, Germany.
authors.forename: Peter
authors.initials: P
authors.lastname: Schmieder
authors.forename: Felix
authors.initials: F
authors.lastname: Nitschke
authors.forename: Martin
authors.initials: M
authors.lastname: Steup
authors.forename: Keven
authors.initials: K
authors.lastname: Mallow
authors.forename: Edgar
authors.initials: E
authors.lastname: Specker
mesh_terms: D002247:Carbon Isotopes; D005936:Glucans / Q000138:chemical synthesis* / Q000737:chemistry; D009682:Magnetic Resonance Spectroscopy / Q000592:standards; D010759:Phosphorus Isotopes; D010766:Phosphorylation; D011522:Protons; D012015:Reference Standards
chemical_list: D002247:Carbon Isotopes; D005936:Glucans; D010759:Phosphorus Isotopes; D011522:Protons
keywords: heteronuclear NMR; phosphorylation; starch; triple resonance