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Chromatographic determination of 1, 4-β-xylooligosaccharides of different chain lengths to follow xylan deconstruction in biomass conversion

  • Hongjia Li
  • Qing Qing
  • Rajeev Kumar
  • Charles E. Wyman
Bioenergy/Biofuels/Biochemicals

Abstract

Xylooligosaccharides released in hydrothermal pretreatment of lignocellulosic biomass can be purified for high-value products or further hydrolyzed into sugars for fermentation or chemical conversion. In addition, characterization of xylooligosaccharides is vital to understand hemicellulose structure and removal mechanisms in pretreatment of cellulosic biomass. In this study, gel permeation chromatography was applied to fractionate xylooligosaccharides produced from birchwood xylan according to their specific degree of polymerization (DP). Then, each fraction was identified by high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) and matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF–MS); and their concentrations were determined by a downscaled post-hydrolysis method. Based on PAD responses and sugar concentrations for each fraction, a series of response factors were developed that can be used to quantify xylooligosaccharides of DP from 2 to 14 without standards. The resulting approach can profile xylooligosaccharides and help gain new insights into biomass deconstruction.

Keywords

Xylooligosaccharides Degree of polymerization HPAEC-PAD Response factor Chromatography 

Notes

Acknowledgments

This research was funded by the BioEnergy Science Center (BESC), a US Department of Energy Bioenergy Research Center supported by the Office of Biological and Environmental Research in the DOE Office of Science. We want to also acknowledge support for some of this research by Mascoma Corporation in Lebanon, NH. The authors especially appreciate Malcolm O’Neil and Trina D. Saffold at the Complex Carbohydrate Research Center of the University of Georgia for MALDI-TOF–MS characterization. We would also like to thank Professor Eugene A. Nothnagel in the Botany and Plant Science Department of the University of California, Riverside for valuable discussion on response factors. Gratitude is extended to the Ford Motor Company for funding the Chair in Environmental Engineering at the Center for Environmental Research and Technology of the Bourns College of Engineering at UCR that augments support for many projects such as this.

References

  1. 1.
    Cantarella M, Cantarella L, Gallifuoco A, Spera A, Alfani F (2004) Effect of inhibitors released during steam-explosion treatment of poplar wood on subsequent enzymatic hydrolysis and SSF. Biotechnol Progr 20(1):200–206. doi: 10.1021/Bp0257978 CrossRefGoogle Scholar
  2. 2.
    Cataldi TRI, Campa C, De Benedetto GE (2000) Carbohydrate analysis by high-performance anion-exchange chromatography with pulsed amperometric detection: the potential is still growing. Fresen J Anal Chem 368(8):739–758CrossRefGoogle Scholar
  3. 3.
    Corradini C, Bianchi F, Matteuzzi D, Amoretti A, Rossi M, Zanoni S (2004) High-performance anion-exchange chromatography coupled with pulsed amperometric detection and capillary zone electrophoresis with indirect ultra violet detection as powerful tools to evaluate prebiotic properties of fructooligosaccharides and inulin. J Chromatogr A 1054(1–2):165–173. doi: 10.1016/j.chroma.2004.07.109 PubMedGoogle Scholar
  4. 4.
    DeLisi C (1980) The biophysics of ligand-receptor interactions. Q Rev Biophys 13(2):201–230PubMedCrossRefGoogle Scholar
  5. 5.
    DeMartini JD, Studer MH, Wyman CE (2011) Small-scale and automatable high-throughput compositional analysis of biomass. Biotechnol Bioeng 108(2):306–312. doi: 10.1002/bit.22937 PubMedCrossRefGoogle Scholar
  6. 6.
    Ebringerova A, Heinze T (2000) Xylan and xylan derivatives—biopolymers with valuable properties, 1-Naturally occurring xylans structures, procedures and properties. Macromol Rapid Comm 21(9):542–556CrossRefGoogle Scholar
  7. 7.
    Gray MC (2005) Heterogeneous dissolution fundamentals for water-only pretreatment of biomass. Dartmouth College, HanoverGoogle Scholar
  8. 8.
    Gray MC, Converse AO, Wyman CE (2007) Solubilities of oligomer mixtures produced by the hydrolysis of xylans and corn stover in water at 180 degrees C. Ind Eng Chem Res 46(8):2383–2391. doi: 10.1021/Ie060325+ CrossRefGoogle Scholar
  9. 9.
    Himmel ME (2008) Biomass recalcitrance: deconstructing the plant cell wall for bioenergy. Blackwell Pub, OxfordCrossRefGoogle Scholar
  10. 10.
    Jensen MB, Johnson DC (1997) Fast wave forms for pulsed electrochemical detection of glucose by incorporation of reductive desorption of oxidation products. Anal Chem 69(9):1776–1781PubMedCrossRefGoogle Scholar
  11. 11.
    Johnson DC (1986) Carbohydrate detection gains potential. Nature 321(6068):451–452CrossRefGoogle Scholar
  12. 12.
    Johnson DC, Lacourse WR (1990) Liquid-chromatography with pulsed electrochemical detection at gold and platinum-electrodes. Anal Chem 62(10):A589–A597Google Scholar
  13. 13.
    Koch K, Andersson R, Aman P (1998) Quantitative analysis of amylopectin unit chains by means of high-performance anion-exchange chromatography with pulsed amperometric detection. J Chromatogr A 800(2):199–206CrossRefGoogle Scholar
  14. 14.
    Koizumi K, Kubota Y, Ozaki H, Shigenobu K, Fukuda M, Tanimoto T (1992) Analyses of isomeric mono-O-methyl-d-glucoses, d-glucobioses and d-glucose monophosphates by high-performance anion-exchange chromatography with pulsed amperometric detection. J Chromatogr 595(1–2):340–345Google Scholar
  15. 15.
    Li X, Converse AO, Wyman CE (2003) Characterization of molecular weight distribution of oligomers from autocatalyzed batch hydrolysis of xylan. Appl Biochem Biotech 105:515–522CrossRefGoogle Scholar
  16. 16.
    Luo C, Brink DL, Blanch HW (2002) Identification of potential fermentation inhibitors in conversion of hybrid poplar hydrolyzate to ethanol. Biomass Bioenergy 22(2):125–138. doi: 10.1016/s0961-9534(01)00061-7 CrossRefGoogle Scholar
  17. 17.
    Paskach TJ, Lieker HP, Reilly PJ, Thielecke K (1991) High-performance anion-exchange chromatography of sugars and sugar alcohols on quaternary ammonium resins under alkaline conditions. Carbohyd Res 215(1):1–14CrossRefGoogle Scholar
  18. 18.
    Rocklin RD, Pohl CA (1983) Determination of carbohydrates by anion exchange chromatography with pulsed amperometric detection. J Liq Chromatogr 6(9):1577–1590CrossRefGoogle Scholar
  19. 19.
    Sluiter A, Hames B, Ruiz R, Scarlata C, Sluiter J, Templeton D (2008) Determination of sugars, byproducts, and degradation products in liquid fraction process samples. Laboratory analytical procedure (LAP), NREL/TP-510-42623. National Renewable Energy Laboratory, Golden, CO, USAGoogle Scholar
  20. 20.
    Studer MH, DeMartini JD, Brethauer S, McKenzie HL, Wyman CE (2010) Engineering of a high-throughput screening system to identify cellulosic biomass, pretreatments, and enzyme formulations that enhance sugar release. Biotechnol Bioeng 105(2):231–238. doi: 10.1002/Bit.22527 PubMedCrossRefGoogle Scholar
  21. 21.
    Timmermans JW, Vanleeuwen MB, Tournois H, Dewit D, Vliegenthart JFG (1994) Quantitative-analysis of the molecular-weight distribution of inulin by means of anion-exchange HPLC with pulsed amperometric detection. J Carbohyd Chem 13(6):881–888CrossRefGoogle Scholar
  22. 22.
    Vazquez MJ, Alonso JL, Dominguez H, Parajo JC (2000) Xylooligosaccharides: manufacture and applications. Trends Food Sci Tech 11(11):387–393CrossRefGoogle Scholar
  23. 23.
    Wyman CE (1999) Biomass ethanol: technical progress, opportunities, and commercial challenges. Ann Rev Energ Env 24:189–226CrossRefGoogle Scholar
  24. 24.
    Wyman CE (2001) Twenty years of trials, tribulations, and research progress in bioethanol technology—selected key events along the way. Appl Biochem Biotech 91–3:5–21CrossRefGoogle Scholar
  25. 25.
    Wyman CE (2007) What is (and is not) vital to advancing cellulosic ethanol. Trends Biotechnol 25(4):153–157. doi: 10.1016/j.tibtech.2007.02.009 PubMedCrossRefGoogle Scholar
  26. 26.
    Yang B, Wyman CE (2008) Characterization of the degree of polymerization of xylooligomers produced by flowthrough hydrolysis of pure xylan and corn stover with water. Bioresource Technol 99(13):5756–5762. doi: 10.1016/j.biortech.2007.10.054 CrossRefGoogle Scholar
  27. 27.
    Zhang YHP, Moxley G (2007) More accurate determination of acid-labile carbohydrates in lignocellulose by modified quantitative saccharification. Energ Fuel 21(6):3684–3688. doi: 10.1021/ef7003893 CrossRefGoogle Scholar

Copyright information

© Society for Industrial Microbiology and Biotechnology 2013

Authors and Affiliations

  • Hongjia Li
    • 1
    • 2
    • 3
  • Qing Qing
    • 1
    • 2
  • Rajeev Kumar
    • 1
    • 2
    • 3
  • Charles E. Wyman
    • 1
    • 2
    • 3
  1. 1.Chemical and Environmental Engineering DepartmentUniversity of California-RiversideRiversideUSA
  2. 2.Center for Environmental Research and TechnologyUniversity of California-RiversideRiversideUSA
  3. 3.BioEnergy Science CenterOak RidgeUSA

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