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Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry
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Combining Fractionation and High-Resolution Mass Spectrometry Approaches to Characterize a Bio-Oil From Flax Shive

Théo Imhoff1,2, Jason Devaux1,2, Estelle Deschamps1,2

  • 1INSA Rouen, INSA Rouen Normandie, Univ Caen Normandie, ENSICAEN, CNRS, Institut CARMeN UMR 6064, Caen, France.

Journal of Separation Science
|January 22, 2026
PubMed
Summary

Flax shive bio-oil molecular complexity was analyzed using size-exclusion chromatography and high-resolution mass spectrometry. This reveals key chemical trends for optimizing bio-oil upgrading and applications in the circular economy.

Keywords:
Fourier‐transform ion cyclotron resonanceOrbitrapbio‐oilfractionationpyrolysis

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Area of Science:

  • Biomass Valorization
  • Green Chemistry
  • Analytical Chemistry

Background:

  • Circular economy and environmental concerns drive innovation in utilizing biomass co-products.
  • Flax industry co-products, like flax shives, are valuable lignocellulosic feedstocks.
  • Pyrolysis of lignocellulosic biomass yields complex, oxygenated bio-oils requiring detailed molecular characterization for effective valorization.

Purpose of the Study:

  • To perform in-depth molecular characterization of bio-oil derived from flax shives.
  • To investigate the influence of size-exclusion chromatography (SEC) fractionation on bio-oil composition.
  • To establish a refined analytical strategy for understanding lignocellulosic bio-oil complexity.

Main Methods:

  • Size-exclusion chromatography (SEC) was employed to fractionate flax shive bio-oil into five distinct fractions.
  • High-resolution mass spectrometry (Fourier-transform ion cyclotron resonance [FT-ICR MS] and Orbitrap MS) was used for molecular formula identification.
  • A custom Python-based workflow was developed for data alignment and annotation, utilizing FT-ICR MS as a reference for Orbitrap MS data.

Main Results:

  • Thousands of molecular formulae were identified and compared across the bio-oil and its SEC fractions.
  • Analysis revealed specific trends in chemical class distribution, oxygen content, and Van Krevelen diagrams across fractions.
  • SEC separation was found to be influenced by molecular size, polarity, and structural interactions, not solely size.

Conclusions:

  • The study successfully characterized the molecular complexity of flax shive bio-oil.
  • The developed analytical approach provides a refined strategy for exploring lignocellulosic bio-oil composition.
  • Findings support future efforts in the upgrading and application of bio-oils within a circular economy framework.