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Characterization of hydrothermally isolated xylan from beech wood by capillary electrophoresis with laser-induced fluorescence and mass spectrometry detection

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Abstract

Hemicelluloses such as xylans play an increasing role as renewable raw materials for technological applications. The complex and variable composition of hemicelluloses requires powerful analytical techniques in order to assess their composition. In the present study, the neutral fraction of hydrothermally isolated xylan from beech wood was characterized by capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) upon derivatization with 8-aminopyrene-1,3,6-trisulfonic acid. Reproducible separation of the xylo-oligosaccharides was achieved using a polyvinyl alcohol coated capillary and a 25 mM sodium acetate buffer, pH 4.75, as background electrolyte at an applied voltage of −30 kV. Intermediate precision expressed as relative standard deviation was below 2.0 % for migration times and below 10 % for relative peak areas except for the oligomers present at very low concentrations only. At the same time, derivatization conditions proved to be robust as well. Samples obtained by fractionation of the xylan were subsequently characterized by CE-LIF. In addition, capillary electrophoresis with mass spectrometry detection indicated the presence of small amounts of xylo-oligosaccharides containing additional sugar moieties such as 4-O-methylglucuronic acid. Moreover, minor components containing acetyl groups could be detected. The presence of these impurities was confirmed by nuclear magnetic resonance analysis of the fractions. In conclusion, although none of the techniques applied here gave a complete picture of the composition of the investigated xylan or its fractions, the combination provided insight into the complexity of the sample.

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Abbreviations

APTS:

8-Aminopyrene-1,3,6-trisulfonic acid

BGE:

Background electrolyte

CE:

Capillary electrophoresis

DMSO:

Dimethyl sulfoxide

DP:

Degree of polymerization

EACA:

ε-Aminocaproic acid

ESI-MS:

Electrospray ionization-mass spectrometry

G:

Gluco-oligomer (numbers indicate degree of polymerization)

HPAEC-PAD:

High performance anion-exchange chromatography with pulsed amperometric detection

HTX:

Hydrothermally treated beech wood xylan

HTX-n:

Neutral fraction of hydrothermally treated beech wood xylan

LIF:

Laser-induced fluorescence

MALDI-MS:

Matrix assisted laser desorption/ionization mass spectrometry

MGA:

4-O-methylglucuronic acid

NMR:

Nuclear magnetic resonance

PGC-ELSD:

Porous graphitized carbon liquid chromatography with evaporative light scattering detection

PVA:

Polyvinyl alcohol

RP-HPLC:

Reversed phase high performance liquid chromatography

RSD:

Relative standard deviation

SEC:

Size-exclusion chromatography

THF:

Tetrahydrofuran

X:

Xylo-oligomer (numbers indicate degree of polymerization)

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Author notes

  1. Pavel Jáč

    Present address: Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 500 05, Hradec Králové, Czech Republic

Authors and Affiliations

  1. Department of Pharmaceutical and Medicinal Chemistry, School of Pharmacy, Friedrich-Schiller University Jena, Philosophenweg 14, 07743, Jena, Germany

    Pavel Jáč & Gerhard K. E. Scriba

  2. Center of Excellence for Polysaccharide Research, Institute of Organic Chemistry and Macromolecular Chemistry, Friedrich-Schiller University Jena, Humboldtstr. 10, 07743, Jena, Germany

    Thomas Elschner, Annett Pfeifer & Thomas Heinze

  3. Bene PharmaChem GmbH & Co. KG, Bayerwaldstr. 7-9, 82538, Geretsried, Germany

    Christian Reiter

  4. Faculty of Chemistry, Aalen University, Beethovenstr. 1, 73430, Aalen, Germany

    Svenja-Catharina Bunz & Christian Neusüß

  5. Orgentis Chemicals GmbH, Bahnhofstraße 3-5, 06466, Gatersleben, Germany

    Hans-Matthias Vorbrodt

Authors
  1. Pavel Jáč
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Correspondence to Pavel Jáč.

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Jáč, P., Elschner, T., Reiter, C. et al. Characterization of hydrothermally isolated xylan from beech wood by capillary electrophoresis with laser-induced fluorescence and mass spectrometry detection. Cellulose 21, 3993–4007 (2014). https://doi.org/10.1007/s10570-014-0456-3

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  • DOI: https://doi.org/10.1007/s10570-014-0456-3

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