Sunday, May 4, 2008
3-19

Evaluation of matrix interference on quantitation of lignocellulosic degradation products in biomass pretreatment samples using LC-ESI-MS/MS

Lekh Nath Sharma1, Bowen Du2, Shishir P. S. Chundawat3, Bruce E. Dale3, and C. Kevin Chambliss1. (1) Chemistry and Biochemistry, Baylor University, One Bear Place #97348, Waco, TX 76798-7348, (2) Environmental Studies, Baylor University, One Bear Place #97266, Waco, TX 76798-7266, (3) Department of Chemical Engineering and Material Science, Michigan State University, 2527 Engineering building, East Lansing, MI 48824

Qualitative and quantitative understanding of potentially inhibitory degradation products produced upon pretreatment of lignocellulosic biomass is paramount to technical and economic valuations of biomass-to-ethanol conversion. Production and release of degradation products results from highly complex chemistry that is poorly understood at this time. Continuing work in our laboratory is focused on using liquid chromatography in combination with electrospray ionization mass spectrometry to monitor accumulation trends of degradation products in biomass pretreatment samples.  The primary analytical advantage of employing mass spectral detection is an unmatched ability to resolve target analytes away from alternative matrix constituents that co-elute chromatographically.  However, successful application of the technique in quantitative analyses requires knowledge of the effect of sample matrix on the analytical response for each target compound.

In the present study, experiments were designed to evaluate matrix interference as a function of various feedstock-pretreatment chemistry combinations. In order to assess the effect of differing feedstocks, dilute acid pretreatments of corn stover and poplar wood were conducted at low, medium, and high severity.  Similar AFEX pretreatments of corn stover were also conducted to assess the effect of varying pretreatment conditions.  Each sample was analyzed using recently developed LC-ESI-MS/MS methodology, and quantitative data derived from an internal standard calibration approach that is subject to matrix effects were compared with data derived using the method of standard additions which compensates for matrix interference.  Results of the study will be presented along with practical guidance on appropriate application of developed methodology for analysis of biomass pretreatment samples.