Detecting Acetylated Aminoacids in Blood Serum using Hyperpolarized 13C-1Η-2D-NMR
authors SotiriosKatsikis, Ildefonso Marin-Montesinos, ChristianLudwig, Ulrich L.Günther
nationality International
journal Journal of Magnetic Resonance
abstract Dynamic Nuclear Polarization (DNP) can substantially enhance the sensitivity of NMR experiments. Among the implementations of DNP, ex-situ dissolution DNP (dDNP) achieves high signal enhancement levels owing to a combination of a large temperature factor between 1.4 and 300K with the actual DNP effect in the solid state at 1.4K. For sufficiently long T1 relaxation times much of the polarization can be preserved during dissolution with hot solvent, thus enabling fast experiments during the life time of the polarization. Unfortunately for many metabolites found in biological samples such as blood relaxation times are too short to achieve a significant enhancement. We have therefore introduced 13C-carbonyl labelled acetyl groups as probes into amino acid metabolites using a simple reaction protocol. The advantage of such tags is a sufficiently long T1 relaxation time, the possibility to enhance signal intensity by introducing 13C, and the possibility to identify tagged metabolites in NMR spectra. We demonstrate feasibility for mixtures of amino acids and for blood serum. In two-dimensional dDNP-enhanced HMQC experiments of these samples acquired in 8 seconds we can identify acetylated amino acids and other metabolites based on small differences in chemical shifts.
year published 2019
volume 305
beginning page 175
digital object identifier (doi) 10.1016/j.jmr.2019.07.003
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