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Detection of potential TNA and RNA nucleoside precursors in a prebiotic mixture by pure shift diffusion-ordered NMR spectroscopy.

Islam S, Aguilar JA, Powner MW, Nilsson M, Morris GA, Sutherland JD - Chemistry (2013)

Bottom Line: One potential avenue is the combination of pure shift methodology, in which NMR spectra are measured with greatly improved resolution by suppressing multiplet structure, with diffusion-ordered spectroscopy, in which NMR signals from different species are distinguished through their different rates of diffusion.Such a combination has the added advantage of working with intact mixtures, allowing analyses to be carried out without perturbing mixtures in which chemical entities are part of a network of reactions in equilibrium.The direct formation of potential RNA and TNA nucleoside precursors, amongst other adducts, was observed.

View Article: PubMed Central - PubMed

Affiliation: School of Chemistry, University of Manchester, Oxford Road, Manchester, M13 9PL, UK. saidul.islam@qmul.ac.uk

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a) Zangger–Sterk pure shift 1H, and b) pure shift 1H DOSY pulse sequences used in the present work. The dark part of the free induction decay represents the component taken from each increment and assembled into a composite interferogram to produce pure shift data, and the grey additional component that was acquired to allow double Fourier transformation for the purposes of multiplicity determination (a previously unreported extension to the experiment). See the main text for details.
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fig03: a) Zangger–Sterk pure shift 1H, and b) pure shift 1H DOSY pulse sequences used in the present work. The dark part of the free induction decay represents the component taken from each increment and assembled into a composite interferogram to produce pure shift data, and the grey additional component that was acquired to allow double Fourier transformation for the purposes of multiplicity determination (a previously unreported extension to the experiment). See the main text for details.

Mentions: The main obstacle to NMR analysis of this type of reaction mixture is lack of resolving power, so it represents an ideal test for a new class of experiment that collapses homonuclear multiplet structure to give a single spectral line per chemical site, and has hence been termed “pure shift” NMR.[31, 33, 41] One of the most effective of these methods for broadband homonuclear decoupling is based on the work of Zangger and Sterk[42] and has been incorporated into a variety of uni- and multidimensional experiments such as DOSY and TOCSY (Figure 3 b).[31, 32, 43] Reported applications of such methods have hitherto been limited to simple samples containing no more than a few chemical species of comparable concentration. Here, Zangger–Sterk methods are applied to a real and highly complex problem in mixture analysis.


Detection of potential TNA and RNA nucleoside precursors in a prebiotic mixture by pure shift diffusion-ordered NMR spectroscopy.

Islam S, Aguilar JA, Powner MW, Nilsson M, Morris GA, Sutherland JD - Chemistry (2013)

a) Zangger–Sterk pure shift 1H, and b) pure shift 1H DOSY pulse sequences used in the present work. The dark part of the free induction decay represents the component taken from each increment and assembled into a composite interferogram to produce pure shift data, and the grey additional component that was acquired to allow double Fourier transformation for the purposes of multiplicity determination (a previously unreported extension to the experiment). See the main text for details.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3814424&req=5

fig03: a) Zangger–Sterk pure shift 1H, and b) pure shift 1H DOSY pulse sequences used in the present work. The dark part of the free induction decay represents the component taken from each increment and assembled into a composite interferogram to produce pure shift data, and the grey additional component that was acquired to allow double Fourier transformation for the purposes of multiplicity determination (a previously unreported extension to the experiment). See the main text for details.
Mentions: The main obstacle to NMR analysis of this type of reaction mixture is lack of resolving power, so it represents an ideal test for a new class of experiment that collapses homonuclear multiplet structure to give a single spectral line per chemical site, and has hence been termed “pure shift” NMR.[31, 33, 41] One of the most effective of these methods for broadband homonuclear decoupling is based on the work of Zangger and Sterk[42] and has been incorporated into a variety of uni- and multidimensional experiments such as DOSY and TOCSY (Figure 3 b).[31, 32, 43] Reported applications of such methods have hitherto been limited to simple samples containing no more than a few chemical species of comparable concentration. Here, Zangger–Sterk methods are applied to a real and highly complex problem in mixture analysis.

Bottom Line: One potential avenue is the combination of pure shift methodology, in which NMR spectra are measured with greatly improved resolution by suppressing multiplet structure, with diffusion-ordered spectroscopy, in which NMR signals from different species are distinguished through their different rates of diffusion.Such a combination has the added advantage of working with intact mixtures, allowing analyses to be carried out without perturbing mixtures in which chemical entities are part of a network of reactions in equilibrium.The direct formation of potential RNA and TNA nucleoside precursors, amongst other adducts, was observed.

View Article: PubMed Central - PubMed

Affiliation: School of Chemistry, University of Manchester, Oxford Road, Manchester, M13 9PL, UK. saidul.islam@qmul.ac.uk

Show MeSH
Related in: MedlinePlus