title: Rapid analysis of carbohydrates in aqueous extracts and hydrolysates of biomass using a carbonate-modified anion-exchange column.
abstract: Quantitative liquid-chromatography techniques used to characterize carbohydrates present in biomass samples can suffer from long analysis times, limited analyte resolution, poor stability, or a combination of these factors. The current manuscript details a novel procedure enabling resolution of glucose, xylose, arabinose, galactose, mannose, fructose, and sucrose via isocratic elution in less than 5 min. Equivalent conditions also enable analysis of cellobiose and maltose with a minimal increase in chromatographic run time (ca. 3 and 6 min, respectively). Noted chromatographic performance requires that a commercially available anion-exchange column be modified with carbonate prior to analysis. Analytical performance of a modified column was assessed over a 5-day period via repeated analyses of 4 samples, resulting from aqueous extraction or quantitative saccharification of a potential biofuel feedstock (i.e., corn stover or switchgrass). A simple solid phase extraction procedure was utilized to clean up each sample prior to analysis. Analytical accuracy of the extraction protocol was assessed by evaluation of matrix spike recoveries which typically ranged from 84% to 98%. The instrumental variability of measured concentrations in real samples over the 5-day period was generally less than 5% RSD for all detected analytes, independent of sample type. Finally, it is important to note that the modified column exhibited exceptional stability over approximately 800 injections of biofeedstock-based samples. These data demonstrate that a carbonate-modified anion-exchange column can be employed for rapid determination of carbohydrates in biomass samples of lignocellulosic origin.
authors.affiliation: Department of Chemistry and Biochemistry, Baylor University, Waco, TX 76798, USA.
authors.forename: Richard S
authors.initials: RS
authors.lastname: Sevcik
authors.forename: Richard A
authors.initials: RA
authors.lastname: Mowery
authors.forename: Christopher
authors.initials: C
authors.lastname: Becker
authors.forename: C Kevin
authors.initials: CK
authors.lastname: Chambliss
mesh_terms: D000838:Anions / Q000737:chemistry; D001673:Biodegradation, Environmental; D056804:Biofuels; D018533:Biomass; D002241:Carbohydrates / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D002254:Carbonates / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D002852:Chromatography, Ion Exchange / Q000379:methods*; D006868:Hydrolysis; D010944:Plants / Q000737:chemistry / Q000378:metabolism; D015203:Reproducibility of Results; D052616:Solid Phase Extraction; D013696:Temperature
chemical_list: D000838:Anions; D056804:Biofuels; D002241:Carbohydrates; D002254:Carbonates