Cellulose

, Volume 21, Issue 6, pp 3993–4007 | Cite as

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

  • Pavel Jáč
  • Thomas Elschner
  • Christian Reiter
  • Svenja-Catharina Bunz
  • Hans-Matthias Vorbrodt
  • Annett Pfeifer
  • Christian Neusüß
  • Thomas Heinze
  • Gerhard K. E. Scriba
Original Paper

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.

Keywords

Xylo-oligosaccharides Reductive amination Capillary electrophoresis Capillary electrophoresis/mass spectrometry Nuclear magnetic resonance 

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)

Supplementary material

10570_2014_456_MOESM1_ESM.pdf (232 kb)
Supplementary material 1 (PDF 231 kb)
10570_2014_456_MOESM2_ESM.pdf (221 kb)
Supplementary material 2 (PDF 220 kb)

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Copyright information

© Springer Science+Business Media Dordrecht 2014

Authors and Affiliations

  • Pavel Jáč
    • 1
    • 6
  • Thomas Elschner
    • 2
  • Christian Reiter
    • 3
  • Svenja-Catharina Bunz
    • 4
  • Hans-Matthias Vorbrodt
    • 5
  • Annett Pfeifer
    • 2
  • Christian Neusüß
    • 4
  • Thomas Heinze
    • 2
  • Gerhard K. E. Scriba
    • 1
  1. 1.Department of Pharmaceutical and Medicinal Chemistry, School of PharmacyFriedrich-Schiller University JenaJenaGermany
  2. 2.Center of Excellence for Polysaccharide Research, Institute of Organic Chemistry and Macromolecular ChemistryFriedrich-Schiller University JenaJenaGermany
  3. 3.Bene PharmaChem GmbH & Co. KGGeretsriedGermany
  4. 4.Faculty of ChemistryAalen UniversityAalenGermany
  5. 5.Orgentis Chemicals GmbHGaterslebenGermany
  6. 6.Department of Analytical Chemistry, Faculty of PharmacyCharles UniversityHradec KrálovéCzech Republic

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