In the Spring of 2013, NMR spectroscopists convened at the Weizmann Institute in Israel to brainstorm on approaches to improve the sensitivity of NMR experiments, particularly when applied in biomolecular settings. This multi-author interdisciplinary Review presents a state-of-the-art description of the primary approaches that were considered. Topics discussed included the future of ultrahigh-field NMR systems, emerging NMR detection technologies, new approaches to nuclear hyperpolarization, and progress in sample preparation. All of these are orthogonal efforts, whose gains could multiply and thereby enhance the sensitivity of solid- and liquid-state experiments. While substantial advances have been made in all these areas, numerous challenges remain in the quest of endowing NMR spectroscopy with the sensitivity that has characterized forms of spectroscopies based on electrical or optical measurements. These challenges, and the ways by which scientists and engineers are striving to solve them, are also addressed.

/pdf/facing-and-overcoming-sensitivity-challenges-in-biomolecular-28nel4u86t.pdf

Facing and Overcoming Sensitivity Challenges in Biomolecular NMR Spectroscopy

Dynamic nuclear polarization (DNP) increases the sensitivity of nuclear magnetic resonance (NMR) spectroscopy by using high frequency microwaves to transfer the polarization of the electrons to the nuclear spins. The enhancement in NMR sensitivity can amount to a factor of well above 100, enabling faster data acquisition and greatly improved NMR measurements. With the increasing magnetic fields (up to 23 T) used in NMR research, the required frequency for DNP falls into the THz band (140- 600 GHz ). Gyrotrons have been developed to meet the demanding specifications for DNP NMR, including power levels of tens of watts; frequency stability of a few megahertz; and power stability of 1% over runs that last for several days to weeks. Continuous gyrotron frequency tuning of over 1 GHz has also been demonstrated. The complete DNP NMR system must include a low loss transmission line; an optimized antenna; and a holder for efficient coupling of the THz radiation to the sample. This paper describes the DNP NMR process and illustrates the THz systems needed for this demanding spectroscopic application. THz DNP NMR is a rapidly developing, exciting area of THz science and technology.

THz Dynamic Nuclear Polarization NMR

Two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy is widely used in chemical and biochemical analyses. Multidimensional NMR is also witnessing increased use in quantitative and metabolic screening applications. Conventional 2D NMR experiments, however, are affected by inherently long acquisition durations, arising from their need to sample the frequencies involved along their indirect domains in an incremented, scan-by-scan nature. A decade ago, a so-called ultrafast (UF) approach was proposed, capable of delivering arbitrary 2D NMR spectra involving any kind of homo- or heteronuclear correlation, in a single scan. During the intervening years, the performance of this subsecond 2D NMR methodology has been greatly improved, and UF 2D NMR is rapidly becoming a powerful analytical tool experiencing an expanded scope of applications. This review summarizes the principles and main developments that have contributed to the success of this approach and focuses on applications that have been recently demonstrated in various areas of analytical chemistry--from the real-time monitoring of chemical and biochemical processes, to extensions in hyphenated techniques and in quantitative applications.

/pdf/ultrafast-2d-nmr-an-emerging-tool-in-analytical-spectroscopy-52c2lk0hfk.pdf

Ultrafast 2D NMR: An Emerging Tool in Analytical Spectroscopy

The role of level anti-crossings in nuclear spin hyperpolarization

A DNP set-up is described where a liquid sample is hyperpolarized by the electron-nucleus Overhauser effect in a field of 034 T and transferred to a field of 1409 T for NMR detection In contrast to a previous set-up, using two dedicated magnets for polarization and detection, a dedicated ferroshim system was inserted into the bore of a 1409 T shielded cryomagnet to provide a homogeneous low-field region in the stray field above the magnetic center After polarization in the low-field the sample is transferred to the high-field magnetic center within 40 ms by a pneumatic shuttle system In our set-up a standard high-resolution inverse 1H/13C selective probe was used for NMR detection and a homebuilt EPR cavity, operating in the TM110 mode was used for polarisation First experimental data are presented We observed a maximum proton Overhauser enhancement of up to eHF = −37 in the high-field position for a 5 mM 4-Oxo-TEMPO-D,15N (TEMPONE)/H2O sample While this reproduces the DNP enhancement observed also in the old set-up, with the new set-up we observe enhancement on larger molecules that were impossible to enhance in the old set-up Therefore, we can demonstrate for the first time Overhauser enhanced high resolution proton spectra of glucose and 2,2-dimethyl-2-silapentane-5-sulfonic acid sodium salt (DSS) in D2O, where the high resolution spectrum was acquired in the high-field position after polarizing the sample in the low-field

/pdf/shuttle-dnp-spectrometer-with-a-two-center-magnet-15ey9ykddc.pdf

Shuttle DNP spectrometer with a two-center magnet

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Shuttle DNP spectrometer with a two-center magnet