Biomass Conversion Research Laboratory, Chemical Engineering and Materials Science, Michigan State University, Lansing, MI 48910, USA.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Apr 15;879(13-14):1018-22. doi: 10.1016/j.jchromb.2011.02.049. Epub 2011 Mar 9.
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.
准确量化木质纤维素生物质热化学预处理过程中形成的反应产物，将有助于更好地理解植物细胞壁的解构，以生产纤维素生物燃料和生物化学品。然而，使用常规液相色谱方法对一些过程副产物（尤其是乙酰胺、乙酸和糠醛）进行定量存在一些分析挑战。因此，我们开发了一种高通量基于气相色谱-质谱联用（GC-MS）的方法，以便在分析之前无需进行耗时的样品衍生化即可定量相关化合物。采用该方法对未经处理、氨纤维膨胀（AFEX）处理和稀酸处理的玉米秸秆的溶剂提取物进行了分析。使用自动溶剂萃取器用丙酮提取生物质样品，连续稀释，并直接使用所提出的 GC-MS 方法进行分析。与水、甲醇和乙腈相比，丙酮是唯一一种不含有可检测到的目标化合物背景水平或在 GC 进样器中促进植物衍生残留物积累的溶剂，这降低了分析重现性。定量结果基于标准添加法和外标校准曲线。
