Relayed-NOE experiments in the rotating frame for sequence analysis of peptides

Kessler, Horst; Gemmecker, Gerd; Haase, Burkhard

doi:10.1016/0022-2364(88)90192-8

Cited by 15 publications

(8 citation statements)

References 13 publications

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“…The analysis of an HMBC spectrum showing intraresidual cross-correlation signals from anomeric protons to carbons C-3 and C-5 was important for the assignment of spin-systems and chemical shifts of carbon. Additionally, long-range correlations between protons of adjacent sugar residues across the glycosidic bond established their sequence; this was confirmed by the analysis of a NOESY spectrum and a 2D-TOCSY-ROESY (TORO) [14][15][16][17] spectrum (Fig. 3).…”

Section: R E S U L T Smentioning

confidence: 73%

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Structural analysis of deacylated lipopolysaccharide of Escherichia coli strains 2513 (R4 core‐type) and F653 (R3 core‐type)

Müller‐Loennies

Lindner

Brade

2002

European Journal of Biochemistry

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Lipopolysaccharide (LPS) of Escherichia coli strain 2513 (R4 core-type) yielded after alkaline deacylation one major oligosaccharide by high-performance anion-exchange chromatography (HPAEC) which had a molecular mass of 2486.59 Da as determined by electrospray ionization mass spectrometry. This was in accordance with the calculated molecular mass of a tetraphosphorylated dodecasaccharide of the composition shown below. NMR-analyses identified the chemical structure as We have also isolated the complete core-oligosaccharides of E. coli F653 LPS for which only preliminary data were available and investigated the deacylated LPS by NMR and MS. The proposed structure determined previously by methylation analysis was confirmed and is shown below.In addition we have quantified the side-chain heptose substitution of the inner core with GlcpN ( 30%) and confirmed that this sugar is only present when the phosphate at the second L,D-Hepp residue is absent.

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Section: R E S U L T Smentioning

confidence: 73%

“…A TORO‐spectrum [14–17] was recorded as a two‐dimensional experiment using a fixed delay as the second mixing time (ROESY‐step). The spectrum was recorded phase‐sensitive by applying TPPI.…”

mentioning

confidence: 99%

Structural analysis of deacylated lipopolysaccharide of Escherichia coli strains 2513 (R4 core‐type) and F653 (R3 core‐type)

Müller‐Loennies

Lindner

Brade

2002

European Journal of Biochemistry

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“…However, interresidue NOES from short flexible peptides are difficult to observe [2,3] due to conformational averaging [4] and an unfavourable correlation time [5]. The influence of the last parameter can be controlled using a solvent of high viscosity [6] or by rotating frame NOE experiments [7,8].…”

Section: Introductionmentioning

confidence: 99%

Nuclear Overhauser effects in aqueous solution as dynamic probes in short linear peptides

Nieto¹,

Jiménez²,

Rico³

et al. 1988

FEBS Letters

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The possibility of obtaining interresidue NOES from short linear peptides in aqueous solution has been investigated from an experimental point of view using peptides of various lengths (namely GGRA, LHRH and RNase S-peptide). It is shown that, provided that long (-800 ms) NOESY mixing times are used, complete sets of sequential aN NOES are obtainable. From the intensities and signs of the observed NOES, the relative mobilities of different parts of the polypeptide chain can be determined.

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“…Further improvements to the procedure are suggested by carrying out the whole experiment in the rotating frame using spin locking pulses. 63 Normally a collection of 2D n.m.r. methods are used to elucidate molecular structures or to assign spectra.…”

Section: Hzmentioning

confidence: 99%

“…63 Normally a collection of 2D n.m.r. This gives rise to unsymmetrical spectra which have been taken advantage of in the sequence determination of polypeptide chains and in resolving assignments which are difficult to make due to overlapping resonances.…”

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confidence: 99%

Chapter 2. Nuclear magnetic resonance spectroscopy

Webb¹

1988

Annu. Rep. Prog. Chem., Sect. C

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IntroductionAs emphasised in previous reports in this series,*-3 any attempt to cover the literature which has appeared over a three year period on a topic as all embracing as n.m.r. spectroscopy must, of necessity, be very selective. The areas chosen for consideration in the present account are similar to those discussed previously'-3 and, thus, are inclined towards some of the more physical topics pertaining to molecular science.Comprehensive accounts of all chemically related fields of n.m.r. investigations are to be found in the Specialist Periodical Reports on n .~. r .~ These volumes contain extensive references to the primary literature and lists of books, reviews and symposia proceedings which provide a means of keeping in contact with recent developments in the n.m.r. technique and its applications.Noteworthy recent advances are included in the present account together with a few key references. An attempt is made to omit those publications which, in the main, represent a hortus conclusus. A glossary of abbreviations used in this chapter is given on page 45. Instrumental Aspects of N.M.R.Developments continue to be reported in various instrumental aspects of n.m.r.. The present account concentrates on some of those relating to pulse sequences, 2D n.m.r. and n.m.r. imaging.A book dealing with the principles of FT n.m.r. has appeared' as well as one covering applications of 1 D and 2D methods to biological systems6 Additional mention may be made of three extensive One of these deals with a coherent theoretical framework for 2D n.m.r. experiments.' The application of 1 D multiple ' G. Figure 1 Schematic representation of screw pulses, in the case of 4 2 phase shifts. Each transition type iies along one of the four axes. The R and L axes carry 'R-type' and Z-type' one-quantum transitions, the P axis carries populations and zero-quantum transitions ('P-type') and the D axis carries double-quantum ('D-type') transitions. It is thus easyto follow the transfer of information among them from left to right (Reproduced with permission from J. Magn. Reson., 1985, 63, 255) pulse techniques to liquids is covered in another review' while the third one provides a comprehensive survey of the various 2D n.m.r. techniques together with a critical account of their applications.'

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Relayed-NOE experiments in the rotating frame for sequence analysis of peptides

Cited by 15 publications

References 13 publications

Structural analysis of deacylated lipopolysaccharide of Escherichia coli strains 2513 (R4 core‐type) and F653 (R3 core‐type)

Structural analysis of deacylated lipopolysaccharide of Escherichia coli strains 2513 (R4 core‐type) and F653 (R3 core‐type)

Nuclear Overhauser effects in aqueous solution as dynamic probes in short linear peptides

Chapter 2. Nuclear magnetic resonance spectroscopy

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