Quantitative rotational-echo double resonance for Carbon-13 spin clusters

Autor: Jacob Schaefer, Gary J. Patti, Miriam Sindelar, Shigeru Matsuoka, Sonal Bansal
Rok vydání: 2021
Předmět:
Zdroj: J Magn Reson
ISSN: 1090-7807
DOI: 10.1016/j.jmr.2021.107043
Popis: By using only half of the total evolution time for dephasing pulses, C{N} rotational-echo double resonance (REDOR) for clusters of (13)C spins (RDX) results in the same universal REDOR behavior as observed for isolated (13)C-(15)N pairs. RDX combines Hahn echoes with solid echoes to suppress interference from scalar J couplings. This is crucial for long evolution times. The modified version (which we call RDX24) makes RDX quantitative for (13)C clusters. We apply this scheme to human embryonic kidney cells labeled in culture by L-[(13)C(5) - (15)N(2)]-glutamine. We quantitatively characterize three separate nitrogen isotopic enrichments for: (i) the alpha nitrogens of glutamine residues in proteins (including the residues of the five amino acids synthesized from glutamine); (ii) the alpha nitrogens of the five amino-acid residues synthesized from glucose, together with those of the nine essential amino acids added to the growth medium; and (iii) the side-chain nitrogens of glutamine (and of asparagine derived from glutamine).
Databáze: OpenAIRE