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A simple fractionation method and GPC analysis of organosolv extracts obtained from lignocellulosic materials

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Abstract

The elucidation of lignin structural features is necessary for the efficient application of this polymer. Fractionation is an effective technique to achieve homogeneous lignin fractions, helping to better understand its composition and structure, and improving its use as source of phenolic compounds. This work develops a new and simple fractionation method of organosolv extracts obtained from lignocellulosic materials that enables the selective separation of lignin (from complex macromolecules to low molecular weight aromatic compounds originated from their degradation) from saccharides derived from hemicelluloses and cellulose. For this purpose, the non-catalytic organosolv extraction of lignin from almond shells was performed with dioxane/water mixtures and then the successful fractionation of the organosolv extracts with anhydrous tetrahydrofuran was achieved, resulting in the selective separation of lignin (lignin fraction) from saccharides (saccharide fraction). Gel permeation chromatography (GPC), thioacidolysis, and GC-MS were used as analytical methods to qualitatively determine the purity of both fractions. In addition, GPC was also used to quantify the content of lignin monomers and furfural in the organosolv extracts, thus allowing valuable information on the state of degradation of the lignin and hemicelluloses extracted to be obtained, respectively. The application of the GPC method also enabled the determination of the molecular weight distribution of the extracted lignin in the same analysis.

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Acknowledgments

This work was supported by the funds of the Green Chemical Process Engineering research group of the University of Murcia (Spain). The authors also would like to thank Ms. Seonaid McNabb for her English revision.

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  1. Department of Chemical Engineering, Faculty of Chemistry, University of Murcia, Campus of Espinardo, 30100, Murcia, Spain

    Pedro Andreo-Martínez, Víctor Manuel Ortiz-Martínez, Nuria García-Martínez, Francisco José Hernández-Fernández, Antonia Pérez de los Ríos & Joaquín Quesada-Medina

  2. Department of Agricultural Chemistry, Faculty of Chemistry, University of Murcia, Campus of Espinardo, 30100, Murcia, Spain

    Pedro Andreo-Martínez & Nuria García-Martínez

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  1. Pedro Andreo-Martínez
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Andreo-Martínez, P., Ortiz-Martínez, V.M., García-Martínez, N. et al. A simple fractionation method and GPC analysis of organosolv extracts obtained from lignocellulosic materials. Biomass Conv. Bioref. 11, 1807–1821 (2021). https://doi.org/10.1007/s13399-019-00593-0

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