Using design of experiments to optimize derivatization with methyl chloroformate for quantitative analysis of the aqueous phase from hydrothermal liquefaction of biomass

Analytical and Bioanalytical Chemistry
René B MadsenMarianne Glasius

Abstract

Hydrothermal liquefaction is a promising technique for the production of bio-oil. The process produces an oil phase, a gas phase, a solid residue, and an aqueous phase. Gas chromatography coupled with mass spectrometry is used to analyze the complex aqueous phase. Especially small organic acids and nitrogen-containing compounds are of interest. The efficient derivatization reagent methyl chloroformate was used to make analysis of the complex aqueous phase from hydrothermal liquefaction of dried distillers grains with solubles possible. A circumscribed central composite design was used to optimize the responses of both derivatized and nonderivatized analytes, which included small organic acids, pyrazines, phenol, and cyclic ketones. Response surface methodology was used to visualize significant factors and identify optimized derivatization conditions (volumes of methyl chloroformate, NaOH solution, methanol, and pyridine). Twenty-nine analytes of small organic acids, pyrazines, phenol, and cyclic ketones were quantified. An additional three analytes were pseudoquantified with use of standards with similar mass spectra. Calibration curves with high correlation coefficients were obtained, in most cases R (2)  > 0.991. Method valid...Continue Reading

References

Dec 1, 1998·Journal of Chromatography. B, Biomedical Sciences and Applications·P Husek
Feb 16, 2012·Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences·D Brynn Hibbert
Jan 1, 2011·Metabolites·Silas G Villas-BôasGeoffrey A Lane

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