Determination of hydroxyl groups in biorefinery resources via quantitative 31 P NMR spectroscopy

Nature Protocols
Xianzhi MengDimitris S Argyropoulos

Abstract

The analysis of chemical structural characteristics of biorefinery product streams (such as lignin and tannin) has advanced substantially over the past decade, with traditional wet-chemical techniques being replaced or supplemented by NMR methodologies. Quantitative 31P NMR spectroscopy is a promising technique for the analysis of hydroxyl groups because of its unique characterization capability and broad potential applicability across the biorefinery research community. This protocol describes procedures for (i) the preparation/solubilization of lignin and tannin, (ii) the phosphitylation of their hydroxyl groups, (iii) NMR acquisition details, and (iv) the ensuing data analyses and means to precisely calculate the content of the different types of hydroxyl groups. Compared with traditional wet-chemical techniques, the technique of quantitative 31P NMR spectroscopy offers unique advantages in measuring hydroxyl groups in a single spectrum with high signal resolution. The method provides complete quantitative information about the hydroxyl groups with small amounts of sample (~30 mg) within a relatively short experimental time (~30-120 min).

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Citations

Jan 24, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Lucía PenínJuan Carlos Parajó
Jul 9, 2020·ChemSusChem·Run-Cang Sun
Jul 18, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Esakkiammal Sudha EsakkimuthuGérard Mortha
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Dec 7, 2021·ACS Sustainable Chemistry & Engineering·Artur BentoCristina Silva Pereira
Dec 10, 2021·Industrial & Engineering Chemistry Research·Xiaojia LuHenrik Grénman

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Methods Mentioned

BETA
NMR
transgenic

Software Mentioned

VnmrJ
Bruker Topspin
SilvaTeam
MestReNova
Topspin

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