Sensitivity- and Gradient-Enhanced Hetero (ω1) Half-Filtered TOCSY Experiment for Measuring Long-Range Heteronuclear Coupling Constants

Dušan Uhrín; Gyula Batta; Victor J. Hruby; Paul N. Barlow; Katalin E. Kövér

doi:10.1006/jmre.1997.1308

Sensitivity- and Gradient-Enhanced Hetero (ω₁) Half-Filtered TOCSY Experiment for Measuring Long-Range Heteronuclear Coupling Constants

Dušan Uhrín, Gyula Batta, Victor J. Hruby, Paul N. Barlow, Katalin E. Kövér

Chemistry and Biochemistry

Research output: Contribution to journal › Article › peer-review

95 Scopus citations

Abstract

An enhanced version of the X(ω₁) half-filtered TOCSY experiment for measurement of long-range heteronuclear coupling constants is proposed which yields high-quality spectra with substantially increased sensitivity and resolution. The modified method features gradient-enhanced X filtering sequences, broadband homonuclear decoupling during t₁, optional ¹J_XII scaling in the F₁ domain, and gradient coherence selection in combination with the sensitivity-enhanced protocol for the TOCSY transfer. These modifications extend the applicability of the method - coupling constants can be measured accurately for natural abundance samples at low concentrations and for compounds yielding complex spectra. Computer-aided analysis of E.COSY-type multiplets is applied for the determination of heteronuclear long-range coupling constants.

Original language	English (US)
Pages (from-to)	155-161
Number of pages	7
Journal	Journal of Magnetic Resonance
Volume	130
Issue number	2
DOIs	https://doi.org/10.1006/jmre.1997.1308
State	Published - Feb 1998

Keywords

Echo-antiecho selection
Gradient-enhanced X filtering
Long-range heteronuclear couplings
Sensitivity enhancement
X(ω) half-filtered TOCSY

ASJC Scopus subject areas

Biophysics
Biochemistry
Nuclear and High Energy Physics
Condensed Matter Physics

Access to Document

10.1006/jmre.1997.1308

Cite this

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title = "Sensitivity- and Gradient-Enhanced Hetero (ω1) Half-Filtered TOCSY Experiment for Measuring Long-Range Heteronuclear Coupling Constants",

abstract = "An enhanced version of the X(ω1) half-filtered TOCSY experiment for measurement of long-range heteronuclear coupling constants is proposed which yields high-quality spectra with substantially increased sensitivity and resolution. The modified method features gradient-enhanced X filtering sequences, broadband homonuclear decoupling during t1, optional 1JXII scaling in the F1 domain, and gradient coherence selection in combination with the sensitivity-enhanced protocol for the TOCSY transfer. These modifications extend the applicability of the method - coupling constants can be measured accurately for natural abundance samples at low concentrations and for compounds yielding complex spectra. Computer-aided analysis of E.COSY-type multiplets is applied for the determination of heteronuclear long-range coupling constants.",

keywords = "Echo-antiecho selection, Gradient-enhanced X filtering, Long-range heteronuclear couplings, Sensitivity enhancement, X(ω) half-filtered TOCSY",

author = "Du{\v s}an Uhr{\'i}n and Gyula Batta and Hruby, {Victor J.} and Barlow, {Paul N.} and K{\"o}v{\'e}r, {Katalin E.}",

note = "Funding Information: This work was, in part (D.U.), supported by the Wellcome Trust. K.E.K. and Gy.B. thank the National Research Foundation and Ministry of Education for financial support (OTKA T 014982, FKFP 0500/1997 to K.E.K. and Gy.B.; OTKA D 23749 to K.E.K.). The purchase of the spectrometer used in the study was supported by OMFB Mec-93-0098, Phare-Accord H-9112-0198, and OTKA A084. The support from NIDA Grant DA 06284 and USPHS Grant DKI7420 is also acknowledged by V.J.H. We thank Dr. J. Hirsch for the sample of the trisaccharide, and S. Liao for the deltorphin analog.",

year = "1998",

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doi = "10.1006/jmre.1997.1308",

language = "English (US)",

volume = "130",

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AU - Batta, Gyula

AU - Hruby, Victor J.

AU - Barlow, Paul N.

AU - Kövér, Katalin E.

N1 - Funding Information: This work was, in part (D.U.), supported by the Wellcome Trust. K.E.K. and Gy.B. thank the National Research Foundation and Ministry of Education for financial support (OTKA T 014982, FKFP 0500/1997 to K.E.K. and Gy.B.; OTKA D 23749 to K.E.K.). The purchase of the spectrometer used in the study was supported by OMFB Mec-93-0098, Phare-Accord H-9112-0198, and OTKA A084. The support from NIDA Grant DA 06284 and USPHS Grant DKI7420 is also acknowledged by V.J.H. We thank Dr. J. Hirsch for the sample of the trisaccharide, and S. Liao for the deltorphin analog.

PY - 1998/2

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N2 - An enhanced version of the X(ω1) half-filtered TOCSY experiment for measurement of long-range heteronuclear coupling constants is proposed which yields high-quality spectra with substantially increased sensitivity and resolution. The modified method features gradient-enhanced X filtering sequences, broadband homonuclear decoupling during t1, optional 1JXII scaling in the F1 domain, and gradient coherence selection in combination with the sensitivity-enhanced protocol for the TOCSY transfer. These modifications extend the applicability of the method - coupling constants can be measured accurately for natural abundance samples at low concentrations and for compounds yielding complex spectra. Computer-aided analysis of E.COSY-type multiplets is applied for the determination of heteronuclear long-range coupling constants.

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