Improved Sensitivity in Gradient-Based 1D and 2D Multiplicity-Edited HSQC Experiments

Parella, Teodor; Sánchez‐Ferrando, Francisco; Virgili, Albert

doi:10.1006/jmre.1997.1164

Cited by 73 publications

(49 citation statements)

References 23 publications

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“…Squared cosine-bell functions were applied in both dimensions and zero-filling was used to expand the data to 512i1024 points. This experiment was slightly modified by the implementation of an editing block in the sequence [26]. The two-dimensional HSQC-TOCSY spectra were recorded with the conventional phase-cycle HSQC pulse sequence concatenated to a WALTZ 16-pulse train with a spin-locking π pulse of 98 µs.…”

Section: Nmr Spectroscopymentioning

confidence: 99%

Structural determination of a 5-acetamido-3,5,7,9-tetradeoxy-7-(3-hydroxybutyramido)-L-glycero-L-manno-nonulosonic acid-containing homopolysaccharide isolated from Sinorhizobium fredii HH103

Gil‐Serrano

Rodrı́guez-Carvajal

Mateo

et al. 1999

Biochemical Journal

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The structure of a polysaccharide from Sinorhizobium fredii HH103 has been determined. This polysaccharide was isolated by following the protocol for lipopolysaccharide extraction. On the basis of monosaccharide analysis, methylation analysis, fast atom bombardment MS, matrix-assisted laser desorption ionization MS, electron-impact high-resolution MS, one-dimensional 1H-NMR and 13C-NMR and two-dimensional NMR experiments, the structure was shown to consist of a homopolymer of a 3:1 mixture of 5-acetamido-3,5,7,9-tetradeoxy-7-[(R)- and (S)-3-hydroxybutyramido]-L-glycero-L-manno-nonulosonic acid. The sugar residues are attached via a glycosidic linkage to the OH group of the 3-hydroxybutyramido substituent and thus the monomers are linked via both glycosidic and amidic linkages. In contrast with the Sinorhizobium K-antigens previously reported, which are composed of a disaccharide repeating unit, the K-antigen polysacharide of S. fredii HH103 is a homopolysaccharide.

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Section: Nmr Spectroscopymentioning

confidence: 99%

Structural determination of a 5-acetamido-3,5,7,9-tetradeoxy-7-(3-hydroxybutyramido)-L-glycero-L-manno-nonulosonic acid-containing homopolysaccharide isolated from Sinorhizobium fredii HH103

Gil‐Serrano

Rodrı́guez-Carvajal

Mateo

et al. 1999

Biochemical Journal

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“…C edited-HSQC spectra [28] were recorded by using z-filter and selection before t1 removing the decoupling during acquisition by use of invigpndph pulse program with CNST2 (JHC) = 145. 2D NOESY experiments were made by using phase-sensitive ge-2D NOESY for CDCl 3 spectra and phase-sensitive ge-2D NOESY with WATERGATE for H 2 O/D 2 O (9:1) spectra.…”

mentioning

confidence: 99%

The Nature and Sequence of the Amino Acid Aglycone Strongly Modulates the Conformation and Dynamics Effects of Tn Antigen's Clusters

Corzana

Busto

Luis

et al. 2009

Chemistry A European J

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Synthetic oligosaccharide vaccines based on carbohydrate epitopes are currently being evaluated as potential immunotherapeutics in the treatment of cancer. In an effort to study the role that the amino acid moiety (L-serine and/or L-threonine residues) plays on the global shape of the resulting glycopeptides and on the dynamics of the carbohydrate moiety, diverse glycopeptides based on the Tn antigen have been synthesized and studied in aqueous solution by combining NMR spectroscopic experiments and molecular dynamics simulations. Our results demonstrate that although the effect of the clustering of Tn on the peptide backbone is not remarkable, it substantially modifies the dynamics, and thus, the presentation features of the carbohydrate moiety. In fact, the selected sequence has a crucial influence on both the orientation and flexibility of the sugar region. Thus, although a serine-threonine pair shows a well-defined spatial disposition of the Tn epitopes, its analogue sequence threonine-serine allows a certain degree of mobility that could favor the interaction with a diversity of receptors without a major energy penalty. These features can be explained by attending to the different conformational behavior of the glycosidic linkage of threonine-containing glycopeptides when compared with those of the serine analogues. On this basis, and taking into account that these carbohydrates interact with components of the immune system, these findings could have implications for further design of new cancer vaccines.

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“…Squared-cosine-bell functions were applied in both dimensions and zero-filling was used to expand the data to 1 K ϫ 1 K. This experiment was slightly modified by the implementation of an editing block in the sequence. [19] The HMBC experiment was performed by using the Bruker standard sequence with 256 increments of 1 K real points to digitize a spectral width of 5682 ϫ 30030 Hz; 64 scans were acquired per increment with a delay of 62.5 ms for evolution of long-range couplings. The ROESY experiment was performed with a mixing time of 300 ms and a relaxation delay between scans of 1.5 s. A data matrix of 256 ϫ 1 K points was used to digitize a spectral width of 5682 Hz; 16 scans were used per increment.…”

Section: Methodsmentioning

confidence: 99%

Structure and Conformational Studies of the Disaccharides Derived from the Inner Core of the Lipopolysaccharide Isolated from Sinorhizobium fredii SMH12

et al. 2008

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The structure and conformational behaviour of the core region of the lipopolysaccharide isolated from Sinorhizobium fredii SMH12, a wide-ranging host bacterium isolated from nodulated soybean plants growing in Vietnam, have been studied. A mixture of oligosaccharides was isolated from the lipopolysaccharide by mild hydrolysis followed by size-exclusion chromatography. The structures were determined by sugar analysis, ESI-MS/MS and NMR studies. Conforma-

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Improved Sensitivity in Gradient-Based 1D and 2D Multiplicity-Edited HSQC Experiments

Cited by 73 publications

References 23 publications

Structural determination of a 5-acetamido-3,5,7,9-tetradeoxy-7-(3-hydroxybutyramido)-L-glycero-L-manno-nonulosonic acid-containing homopolysaccharide isolated from Sinorhizobium fredii HH103

Structural determination of a 5-acetamido-3,5,7,9-tetradeoxy-7-(3-hydroxybutyramido)-L-glycero-L-manno-nonulosonic acid-containing homopolysaccharide isolated from Sinorhizobium fredii HH103

The Nature and Sequence of the Amino Acid Aglycone Strongly Modulates the Conformation and Dynamics Effects of Tn Antigen's Clusters

Structure and Conformational Studies of the Disaccharides Derived from the Inner Core of the Lipopolysaccharide Isolated from Sinorhizobium fredii SMH12

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