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(SE)-E-3-E.COSY methods for the measurement of F-19 associated scalar and dipolar coupling constants

  1. Author:
    Luy, B.
    Barchi, J. J.
    Marino, J. P.

  2. Author Address

    Univ Maryland, Ctr Adv Res Biotechnol, 9600 Gudelsky Dr, Rockville, MD 20850 USA. Univ Maryland, Ctr Adv Res Biotechnol, Rockville, MD 20850 USA. NIST, Rockville, MD 20850 USA. NCI, Med Chem Lab, FCRDC, Frederick, MD 21702 USA. Marino JP Univ Maryland, Ctr Adv Res Biotechnol, 9600 Gudelsky Dr, Rockville, MD 20850 USA.
    1. Year: 2001
  2. Journal: Journal of Magnetic Resonance
    1. 152
    2. 1
    3. Pages: 179-184
  4. Type of Article: Article
  1. Abstract:

    A H-1-F-19 spin state selective excitation ((SE)-E-3) pulse sequence element has been applied in combination with IH homonuclear mixing to create E.COSY-type experiments designed to measure scalar J(HF2') and J(HH2') and residual dipolar D- HF2' and D-HH2' couplings in 2'-deoxy-2'-fluoro-sugars. The H- 1-F-19 (SE)-E-3 pulse sequence element, which resembles a simple INEPT sequence, achieves spin-state-selective correlation between geminal H-1-F-19 spin pairs by linear combination of in-phase F-19 magnetization and anti-phase magnetization evolved from H-1. Since the (SE)-E-3 sequence converts both F-19 and H-1 steady-state polarization into observable coherences, an approximately twofold signal increase is observed for fully relaxed H-1-F-19 spin pairs with respect to a standard H-1 coupled F-19 1D experiment. The improved sensitivity and resolution afforded by the use of H-1-F-19 (SE)-E-3 E.COSY-type experiments for measuring couplings is demonstrated on the nucleoside 9-(2',3'-dideoxy-2'-fluoro-beta -D-threo-pentofuranosyl)adenine (beta -FddA) and on a selectively 2'-fluorine labeled 21mer RNA oligonucleotide.

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