High-precision heteronuclear 2D NMR experiments using 10-ppm spectral window to resolve carbon overlap

Vitorge, Bruno; Bieri, Stefan; Humam, Munir; Christen, Philippe; Hostettmann, Kurt; Muñoz, Orlando; Loss, Sandra; Jeannerat, Damien

doi:10.1039/b820478k

Cited by 34 publications

(27 citation statements)

References 14 publications

(4 reference statements)

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“…For example, in the case of an aliased spectrum with an F1 scale covering 5 to 6 ppm, a signal normally found at 1.234 ppm will be located at 5.234 ppm in the aliased spectrum. [16] The fact that accidental overlap may occur when pairs of signals accidentally share the same last digits (for example a signal at 3.234 ppm) sometimes requires a complementary spectrum to be recorded with a slightly different window (say 1.05 ppm) to insure that pairs of signals overlapping in the first spectrum will not overlap in the second. [17] The same principle can be applied to a 100-fold reduction of the number of time increments with a window of 0.1 ppm.…”

Section: Combination With Spatial Encoding Methodologymentioning

confidence: 99%

“…The fact that 13 C are easily decoupled at natural abundance and produce narrow singlets explains why most applications of aliasing techniques were focused on the 13 C dimension of heteronuclear experiments. [14][15][16] When the scalar coupling patterns are complex, as in 1 H spectra, but also in 13 C-enriched compounds, [17] homonuclear decoupling is necessary to create enough space between the signals to permit aliased signals to fit in between. Even if 1 H spectra are about five times narrower than 13 C when measured in Hz, the potential of improvement of the resolution is quite interesting.…”

Section: Combination With Spatial Encoding Methodologymentioning

confidence: 99%

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Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

Cotte

Foroozandeh

Jeannerat

2012

Chimia

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Broadband homonuclear decoupling (BBHD) in the indirect 1 H dimension of 2D experiments can be obtained using a modified Zangger and Sterk combination of a selective pulse with a pulsed-field gradient. The coupling structure of signals is reduced to a singlet along the F1 dimension at the cost of a sensitivity loss. With the classical sampling in F1, the full resolving power of BBHD-experiments requires very long acquisition times. Spectral aliasing can reduce the number of time increments accessing the top resolution of homodecoupled spectra of small molecules by two orders of magnitude. The TOCSY spectra of androst-4-ene-3,17-dione are shown as an example.

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Section: Combination With Spatial Encoding Methodologymentioning

confidence: 99%

Section: Combination With Spatial Encoding Methodologymentioning

confidence: 99%

Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

Cotte

Foroozandeh

Jeannerat

2012

Chimia

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“…Signal assignment was clearly facilitated by the availability of the coupling constants.K nowing that all couplings above 9Hzare geminal (12)(13)(14)(15)(16)(17)(18)(19)(20) Hz in the case of androsten) or trans diaxial (9)(10)(11)(12)(13)(14)(15), the visual inspection of the couplings …”

Section: Methodsmentioning

confidence: 99%

1D NMR Homodecoupled ¹H Spectra with Scalar Coupling Constants from 2D NemoZS‐DIAG Experiments

Cotte

Jeannerat

2015

Angew Chem Int Ed

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A two-dimensional liquid-state NMR experiment cleanly separating chemical shifts and scalar couplings information is introduced. This DIAG experiment takes advantage of a drastic reduction of the spectral window in the indirect dimension to be quickly recorded and of a new non-equidistant modulation of the selective pulse to improve the sensitivity of the broadband homodecoupling Zangger-Sterk sequence element by one order of magnitude. A simple automatic analysis results in 1D spectra displaying singlets and lists of the scalar couplings for first-order multiplets. This facilitates the analysis of 1D spectra by resolving multiplets based on their differences in chemical shifts and coupling structures.

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“…As mentioned in paragraph 2, various approaches have been proposed to overcome these drawbacks without degrading the SNR and the resolution. The simplest one consists in classical peak aliasing along the conventional dimension . However, this strategy is not applicable in the spatially encoded dimension where no FT is applied.…”

Section: Spectral Width Improvementsmentioning

confidence: 99%

Fast hybrid multi‐dimensional NMR methods based on ultrafast 2D NMR

Akoka

Giraudeau

2015

Magnetic Reson in Chemistry

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Conventional multi-dimensional (nD) NMR experiments are characterized by inherent long acquisition durations, while ultrafast (UF) NMR makes it possible to reduce to a few hundreds of milliseconds the overall acquisition duration of a complete nD NMR dataset. Although extremely promising for a number of specific applications, the UF strategy suffers from significant limitations compared with its conventional counterpart. The main limitations concern the sensitivity, the resolution, and the accessible spectral width. However, when the targeted applications are compatible with an acquisition duration between a few seconds and a few minutes, hybrid UF techniques can be used to improve the performance of UF nD NMR while remaining faster than conventional acquisitions. Much better results in terms of signal-to-noise ratio can be achieved with the multi-scan single-shot approach or with interleaved acquisitions. Even more, for the same experimental duration, and in the case of homonuclear 2D NMR, the multi-scan single-shot approach has a much higher precision than conventional 2D NMR. Interleaved 2D NMR overcomes the drawbacks of single-scan UF NMR in terms of spectral width and provides spectra for which the quality is not significantly different from that obtained with conventional 2D NMR. Finally, high spectral qualities have been demonstrated from hybrid conventional/UF 3D approaches capable of recording a whole 3D spectrum in the time needed to record a conventional 2D spectrum. This mini-review aims at describing the principles, the recent advances and the latest applications of these hybrid techniques. Copyright © 2015 John Wiley & Sons, Ltd.

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High-precision heteronuclear 2D NMR experiments using 10-ppm spectral window to resolve carbon overlap

Abstract: The acquisition of a complementary heteronuclear 2D NMR experiment with 10-ppm carbon window allows chemists to improve by a factor 20-25 the spectral resolution and determine carbon chemical shifts with five figures from 2D spectra.

Cited by 34 publications

References 14 publications

Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

1D NMR Homodecoupled ¹H Spectra with Scalar Coupling Constants from 2D NemoZS‐DIAG Experiments

Fast hybrid multi‐dimensional NMR methods based on ultrafast 2D NMR

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High-precision heteronuclear 2D NMR experiments using 10-ppm spectral window to resolve carbon overlap

Abstract: The acquisition of a complementary heteronuclear 2D NMR experiment with 10-ppm carbon window allows chemists to improve by a factor 20-25 the spectral resolution and determine carbon chemical shifts with five figures from 2D spectra.

Cited by 34 publications

References 14 publications

Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

Combination of Homonuclear Decoupling and Spectral Aliasing to Increase the Resolution in the 1H Dimension of 2D NMR Experiments

1D NMR Homodecoupled 1H Spectra with Scalar Coupling Constants from 2D NemoZS‐DIAG Experiments

Fast hybrid multi‐dimensional NMR methods based on ultrafast 2D NMR

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1D NMR Homodecoupled ¹H Spectra with Scalar Coupling Constants from 2D NemoZS‐DIAG Experiments