ST1-02: Rapid HPAE-PAD determination of sugars in liquid process samples: Inter-laboratory comparion of analytical performance for the CarboPac SA10 stationary phase

Wednesday, May 4, 2011: 7:20 PM
Grand Ballroom A, 2nd fl (Sheraton Seattle)
C. Kevin Chambliss1, Richard S. Sevcik1, Deborah A. Hyman2, Christopher J. Scarlata2 and Chris Pohl3, (1)Department of Chemistry and Biochemistry, Baylor University, Waco, TX, (2)National Bioenergy Center-Biomass Analysis Team, National Renewable Energy Laboratory, Golden, CO, (3)R&D, Dionex Corporation, Sunnyvale, CA
Analyses of carbohydrates present in liquid process samples or solvent extracts derived from biomass have typically relied on chromatographic protocols that are either time consuming, offer limited analyte resolution, or both.  Our group has previously demonstrated that near-baseline resolution of sucrose and monomeric sugars common to biomass samples could be achieved in approximately 5 min when a carbonate-modified anion-exchange column was utilized.  Inspired by our approach, Dionex Corporation has more recently developed a commercially-available stationary phase (CarboPac SA10) that offers comparable chromatographic performance (near-baseline resolution of sucrose, arabinose, galactose, glucose, xylose, mannose, and fructose in less ca. 7 minutes when 1 mM KOH is employed as an isocratic mobile phase), yet alleviates the need for column modification.  Additionally, use of a low-volume injection valve in combination with a large-volume spacer in the electrochemical detector block has minimized the usual caveat of having to analyze biomass samples at high dilution when pulsed amperometric detection (PAD) is employed.  In the present study, the HPAE-PAD approach was utilized to interrogate sugars present in a variety of liquid process samples (e.g., aqueous extracts and liquid samples derived from pretreatment, enzymatic hydrolysis, and SSF of biomass).  A subset of these samples was evaluated by analysts and instrumentation from independent laboratories.  Presented data will seek to define the ruggedness characteristics of the SA10 stationary phase, as well as, provide a robust comparison of intra- and inter-laboratory precision and accuracy metrics that enable assessment of method transfer characteristics of the technique.