The selective 1D COSY experiment permit to obtain 1D
COSY spectra from which COSY patterns can be easily extracted and analyzed
in terms of coupling constant values. Improved results are obtained from
the gradient-based selective ge-1D
COSY experiment.
REQUIREMENTS
Easy implementation on AVANCE spectrometers with selective
excitation using shaped pulses.
VERSIONS
The selective ge-1D COSY experiment consists of three parts:
Evolution of
homonuclear J-couplings during an optimized delay followed by a mixing
90º pulse for anti-phase polarizationtransfer to other spins
(see COSY Block).
The first published version of the selective 1D COSY experiment
(
86JMR106-70
)
used a single (90º or 270º) gaussian pulse as a selective excitation.
A DANTE pulse train
(
96CONC119
)
has also been used.
Addition of a refocusing delay and a Z-filter just prior to acquisition
(
86JMR106-70
)
in order to achieve in-phase magnetization.
Using a chemical-shift-selective filter (CSSF)
(
88JMR548-76
,
88JMR582-78
, and
91TET3535
).
Using the DICE approach
(
90JMR331-87
).
Using the TSE-TSE (double-resonance two-spin effect) scheme
(
94JMRA246-107
,
95JMRA72-112
,
95JMRA273-116
,
95JMRA128-117
,
96JMRA90-119
, and
96JMRA145-119
).
The TSETSE experiments offer a new form of correlation spectroscopy
by applying two simultaneous soft pulses at two different chemical sites,
converting in-phase absorption-mode magnetization into anti-phase dispersion-mode
magnetization.
A selective 1D 13C COSY experiment has also been applied to
13C-labeled compounds
(
90MRC149
).
EXPERIMENTAL DETAILS
The selective 1D COSY experiment can be run with minor changes
from a predefined parameter set. Detailed description of the experiment
can be found in the original publication
(
86JMR106-70
).
Two important parameters to consider are:
Selectivity of the selective excitation pulse:
the user must define the shape, the duration and the power level needed
for a defined excitation profile.
Optimization of the J-coupling delay
as a function of 1/(2*J(HH)), in order to get the anti-phase magnetization
of the selected proton suitable for transfer polarization.
In 1D COSY spectra, all coupled protons appear in antiphase
pattern with respect to the active coupling of the selected proton and
in-phase pattern with respect to all other passive couplings.