Sunday, May 4, 2008
3-34

Rapid high performance liquid chromatography analysis of sugars in aqueous extracts and dilute-acid hydrolysates of herbaceous biomass

Richard S. Sevcik, Richard A. Mowery, and C. Kevin Chambliss. Chemistry and Biochemistry, Baylor University, One Bear Place Box #97348, Waco, TX 76706

An improved high performance liquid chromatography (HPLC) method for determination of biomass sugars in aqueous samples has been developed and validated.  The method employed a commercially-available anion-exchange column that was modified with sodium carbonate prior to sample analysis, and the modified column resulted in baseline resolution of sucrose, arabinose, galactose, glucose, xylose, mannose, fructose, and an internal standard in approximately 5 minutes.  Eluted compounds were detected using pulsed amperometry, and the observed linear response for each analyte resulted in statistically-dervied limits of detection (S/N = 3) and quantitation (S/N = 10) ranging from 0.89-2.51 µg/L and 2.87-7.98 µg/L, respectively.  Method precision was evaluated by analyzing an aqueous extract and a dilute-acid hydrolysate, derived from both corn stover and switchgrass materials, over a five-day period.  Observed retention times varied by <1% after more than 800 sample injections, and inter- and intra-day precision, measured as the relative standard deviation of individual analyte concentrations, ranged from 2-13% and 4-12%, respectively, independent of sample type.  Additionally, analysis of matrix spike samples resulted in analyte recoveries ranging from 79-106%, demonstrating excellent accuracy. These data clearly demonstrate the utility of developed methodology for analysis of biomass samples. 

 


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