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Selective ge-1D HSQC-COSY

DESCRIPTION
The selective ge-1D HSQC-COSY experiment allows to obtain high-quality 1D HSQC-COSY spectra from which 1H-1H J-correlation can be elucidated starting from a selected carbon. Thus, in the first part of this experiment, magnetization is transferred from the selected carbon to the directly-bonded protons via a selective HSQC block. After this, the in-phase magnetization of these protons is allowed to evolve by a conventional COSY block under the effect of homonuclear J(HH) coupling. The same principles described here are also applied to the selective ge-1D HMQC-COSY experiment.

REQUIREMENTS
Easy implementation on AVANCE spectrometers equipped with pulsed field gradients, selective excitation using shaped pulses and inverse probehead.
VERSIONS
The basic pulse sequence of the selective ge-1D HSQC-COSY experiment is exactly the same as the conventional ge-2D HSQC-COSY pulse train in which the following modifications have been included ( 95JMRA32-114 ):
A related 2D experiment was proposed (ge-2D selective-HSQC-COSY experiment) in which COSY cross-peaks can be detected and evaluated in overcrowded regions ( 95MRC144 ).
EXPERIMENTAL DETAILS
The selective ge-1D HSQC-COSY experiment can be run with minor changes from a predefined parameter set. The HSQC block is optimized as discussed in the selective ge-1D HSQC experiment and the COSY delay is optimized as usual. Important parameters to consider are:
  • Selectivity of the selective excitation 13C pulse: the user must define the offset, the shape, the duration and the power level needed for a defined excitation profile.
  • Optimization of the J-coupling delay in the HSQC block as a function of 1/(4*J(CH)), in order to get in-phase magnetization of the directly-bonded protons.
  • Optimization of the J-coupling delay in the COSY block as a function of 1/(2*J(HH)), in order to get antiphase magnetization of all protons J-coupled with the directly-attached proton.
  • SPECTRA
    The selective ge-1D HSQC-COSY experiment affords a simple 1D 13C-edited COSY spectrum in which the  protons directly-bonded to the selected carbon appear as large doublet due to 1JCH and the protons J-coupled with them show the commonly anti-phase pattern of COSY signals. The use of gradients allows to obtain a clean, artefact-free spectrum in a short time in which perfect suppression of undesired 1H-12C magnetization is achieved with a single two-step phase cycle (the selective 90º carbon pulse and the receiver are usually inverted on alternated scans).
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