New practical tools for the implementation and use of ultrafast 2D NMR experiments

Abstract

Ultrafast (UF) 2D NMR is a very promising methodology enabling the acquisition of 2D spectra in a single scan. In the last few years, the analytical performance of UF 2D NMR has been highly increased, consequently maximizing its range of applications. However, its implementation and use by non-specialists are far from being straightforward, because of the specific acquisition and processing procedures and parameters characterizing UF NMR. To make this methodology implementable and applicable by non-specialists, we developed a simple routine capable of translating conventional parameters (spectral widths and transmitter frequencies) into specific UF parameters (gradient and chirp pulse parameters). This macro was subsequently implemented in a Web page, which is available for external users. Although the algorithm was designed for two widely used 2D experiments, COSY and HSQC, it can easily be extended to any other pulse sequence. The robustness of this routine was verified successfully on a variety of small molecules. We believe that this tool will eliminate much of the technical difficulties related to UF 2D NMR and will make the technique accessible to a wider audience of organic and analytical chemists.

Quantitative 2D liquid‐state NMR

“…Based on this higher performance, we recently applied the M3S COSY experiment to determine, with high precision, the absolute concentration of metabolites in breast cancer cell lines (Fig. ) . High accuracy was ensured thanks to a standard addition approach.…”

Monitoring organic reactions by UF‐NMR spectroscopy

“…Recent advances in UF‐NMR make it possible to implement it with a standard NMR spectrometer. Additionally, in comparison to the standard NMR, the protocols already described by Patrick Giraudeau provide an easy access to the performance of the necessary additional operations. The complete information about the routines and programs we applied is also available .…”

Reverse detection for spectral width improvements in spatially encoded dimensions of ultrafast two-dimensional NMR spectra

“…Regarding the rest of the experimental parameters, it is instructive to refer to the previous work [26] by Giraudeau and coworkers.…”

“…The value of m is determined by its corresponding one‐dimensional (1D) spectrum, and the amplitude and duration of the skipping gradient can then be chosen according to the formula . Regarding the rest of the experimental parameters, it is instructive to refer to the previous work by Giraudeau and coworkers.…”