Sakhaii Peyman, Bohorc Bojan, Schliedermann Uwe, Berchtold Harald, Bermel Wolfgang
NMR Laboratory of SANOFI, TIDES Analytical Sciences / German NMR Platform Industriepark Hoechst, Building G849, D-65926 Frankfurt/Main, Germany.
Bruker BioSpin GmbH, Silberstreifen, D-76287 Rheinstetten, Germany.
J Magn Reson. 2020 Jun;315:106753. doi: 10.1016/j.jmr.2020.106753. Epub 2020 May 15.
A new experiment for recording phase sensitive ω-broadband homodecoupled TOCSY spectra is presented. The method is an extension of the already existing perfect echo (PE) filter, proposed to sample t chemical shift under sustained homodecoupling. The modification is made by attaching a time reversed perfect echo filter to a regular perfect echo scheme. Thus it becomes possible to acquire for longer t acquisition times without compromising the quality of homodecoupling. The mirror symmetric double perfect echo is implemented into the evolution period of a TOCSY experiment. A spin lock pulse purges undesired dispersive antiphase components at the end of the central t evolution period. Pure absorptive lineshapes with reduced proton spin multiplicities are obtained. The approach can be used in conjunction with real or constant time chemical shift evolution. In case of compounds with reduced T relaxation time, the real time approach is advisable, where the echo delays are an extension of the t evolution period. In this way, an unnecessary loss due to T relaxation is avoided. Using the pulse sequence in constant time mode at high t values gives ω-homodecoupled TOCSY spectra without a significant dependence of the transfer amplitude on J. All experiments were carried out using non uniform sampling to decrease the measurement time. Experimental setup, advantages and limitations are discussed.