title: Rapid quantification of major reaction products formed during thermochemical pretreatment of lignocellulosic biomass using GC-MS.
abstract: Accurate quantification of reaction products formed during thermochemical pretreatment of lignocellulosic biomass would lead to a better understanding of plant cell wall deconstruction for production of cellulosic biofuels and biochemicals. However, quantification of some process byproducts, most notably acetamide, acetic acid and furfural, present several analytical challenges using conventional liquid chromatography methods. Therefore, we have developed a high-throughput gas chromatography based mass spectrometric (GC-MS) method in order to quantify relevant compounds without requiring time-consuming sample derivatization prior to analysis. Solvent extracts of untreated, ammonia fiber expansion (AFEX) treated and dilute-acid treated corn stover were analyzed by this method. Biomass samples were extracted with acetone using an automated solvent extractor, serially diluted and directly analyzed using the proposed GC-MS method. Acetone was the only solvent amongst water, methanol and acetonitrile that did not contain detectable background levels of the target compounds or facilitate a buildup of plant-derived residues in the GC injector, which decreased analytical reproducibility. Quantitative results were based on the method of standard addition and external standard calibration curves.
authors: Biomass Conversion Research Laboratory, Chemical Engineering and Materials Science, Michigan State University, Lansing, MI 48910, USA. humpulaj@egr.msu.edu
authors: James F
authors: JF
authors: Humpula
authors: Shishir P S
authors: SP
authors: Chundawat
authors: Ramin
authors: R
authors: Vismeh
authors: A Daniel
authors: AD
authors: Jones
authors: Venkatesh
authors: V
authors: Balan
authors: Bruce E
authors: BE
authors: Dale
mesh_terms: D000081:Acetamides; D019342:Acetic Acid; D000096:Acetone / Q000737:chemistry*; D000097:Acetonitriles; D056804:Biofuels; D018533:Biomass; D005662:Furaldehyde; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D057166:High-Throughput Screening Assays; D006358:Hot Temperature; D008031:Lignin / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D000432:Methanol; D012044:Regression Analysis; D015203:Reproducibility of Results; D014867:Water; D003313:Zea mays
chemical_list: D000081:Acetamides; D000097:Acetonitriles; D056804:Biofuels; D014867:Water; C036909:lignocellulose; D000096:Acetone; C030686:acetamide; D008031:Lignin; D005662:Furaldehyde; D019342:Acetic Acid; D000432:Methanol; C032159:acetonitrile