Measuring couplings in crowded NMR spectra: pure shift NMR with multiplet analysis

Abstract

The PSYCHE method for pure shift NMR is exploited to generate 2D J spectra with full decoupling in one dimension and multiplet structure in the other, allowing spin-spin coupling constants to be measured even in very crowded spectra. Significant improvements over existing techniques are demonstrated for the hormones estradiol and androstenedione.

Probing Long‐Range Anisotropic Interactions: a General and Sign‐Sensitive Strategy to Measure 1H–1H Residual Dipolar Couplings as a Key Advance for Organic Structure Determination

“… a) Structure of (+)‐IPC; b) isotropic 1D 1 H spectrum in CD 2 Cl 2 ; c) TSE‐PSYCHE pure shift spectrum in CD 2 Cl 2 (isotropic); d) anisotropic 1D 1 H spectrum in PBDG/CD 2 Cl 2 ; e) TSE‐PSYCHE pure shift spectrum in PBDG/CD 2 Cl 2 (anisotropic). For each segment in the spectra, intensities were scaled as shown.…”

Pure shift 1H NMR: what is next?

“…[21,22,25,[48][49][50][51][52][53][54][55] Further promising applications are currently in their initial stage of development, such as the combination of pure shift with the dynamic nuclear polarization technique [56] or the use of pure shift spectra to carry out quantitative studies in metabolomics. [57] In the future, it could also be possible to explore the application of pure shift techniques to other nuclei (such as 19 F, 31 P or 2 H), in quality control processes, drug degradation studies and to monitor fast reactions, among others. Additionally, the use of pure chemical shift data also opens up new possibilities to carry out structure elucidation and verify molecular structures in an automatic way by using for example computer-assisted structure elucidation programs.…”

Real-time bilinear rotation decoupling in absorptive mode J-spectroscopy: Detecting low-intensity metabolite peak close to high-intensity metabolite peak with convenience

“…Recently, we have replaced these multiplets by singlets in F 2 by applying real-time BASH decoupling improving resolution and sensitivity of the technique in a band selective manner [30]. Triple Spin Echo (TSE) PSYCHE 2D Jsequence is another approach reported very recently to produce absorption mode J-spectrum with pure shift spectrum in F 2 and J-coupling information along F 1 [31]. The method is based on Pell and Keeler method [24] and utilizes PSYCHE J-refocusing pulse element to reverse the sense of t 1 evolution in 2D J-spectroscopy.…”