Monday, April 19, 2010
2-21

Characterization and semiquantitative estimation of biomass recalcitrance in switchgrass by whole cell HSQC analysis in perdeuterated pyridinium chloride/DMSO-d6  solvent system

Reichel S*, Marcus F, Nan J, Arthur J. Ragauskas, School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlantic Dr, 10 thArthur, Atlanta, GA 30332

Switchgrass is being considered as a sustainable bio-energy crop due to its broad adaptability, high mass yield, low agricultural input and positive environmental effects.  Its current conversion to biofuels is detrimentally impacted by its recalcitrance which is addressed using chemical and/or biological pretreatments. Lignin–carbohydrate associations are the cause of natural recalcitrance in biomass. Extensive research is ongoing to study the fundamental structural components contributing to recalcitrance and how this can be minimized.  Traditional methodologies used for the characterization plant biopolymers contributing to recalcitrance typically involve lengthy isolation protocols followed by characterization with advanced spectroscopic techniques. Recently, our group has developed an ionic liquid solvent system, perdeuterated pyridinium chloride-DMSO, for the dissolution of whole biomass and followed by NMR analysis. We have employed this methodology for the characterization and estimation of structural changes during pretreatment of biomass. In this study, extractives free switchgrass was pretreated at neutral, acidic and basic conditions at 170 oC.  Wiley milled pretreated  samples were dissolved in perdeuterated pyridinium chloride –DMSO-d6 solvent system and 13C-1H HSQC NMR  spectra  were recorded. This data was semi-quantitatively analyzed by estimating the volume integral of the resolved lignin and hemicellulose cross peaks which can be used to easily monitor the structural changes in switchgrass caused by pretreatment.