Fractionation by flash chromatography and molecular characterization of bio-oil by ultra-high-resolution mass spectrometry and NMR spectroscopy

• Published in: Journal of analytical and applied pyrolysis Vol. 166; p. 105611
• Main Authors: Hertzog, Jasmine, Garnier, Carole, Mase, Charlotte, Mariette, Sandra, Serve, Olivier, Hubert-Roux, Marie, Afonso, Carlos, Giusti, Pierre, Barrère-Mangote, Caroline
• Format: Journal Article
• Language: English
• Published: Elsevier B.V 01.09.2022; Elsevier
• Subjects: Analytical chemistry; Bio-oil; Chemical Sciences; Environmental Sciences; Flash chromatography; Fractionation; FT-ICR MS; NMR; Fractionation; NMR; FT-ICR MS; Flash chromatography; Bio-oil
• ISSN: 0165-2370; 1873-250X
• DOI: 10.1016/j.jaap.2022.105611

Bio-oils obtained from the pyrolysis of lignocellulosic biomass are highly complex matrices with tens of thousands of organic compounds covering a wide polarity and mass range. Their upgrading into greener fuel or value-added chemicals requires an in-depth knowledge of their molecular composition prior and after valorization treatment, which can be obtained by different analytical techniques. Here, flash chromatography was employed as an efficient way to fractionate a bio-oil vacuum residue into four distinct fractions. This process was repeatable at both gravimetric and chromatographic levels and provided information about the weight contribution of each fraction to bio-oil composition. Achieved fractions were then characterized by ultra-high-resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) and nuclear magnetic resonance spectroscopy. These two techniques ensured the good repeatability of bio-oil fractionation at the molecular level and also highlighted molecular specificities of each fraction. Thus, flash chromatography provided quantitative information that was complementary to FT-ICR MS results. It also simplifies the bio-oil compositional analysis, making it possible to detect more compounds. Eventually, this fractionation process can also be used to target fraction or compounds of interest for bio-oil upgrading. [Display omitted] •Flash chromatography is a repeatable method for bio-oil fractionation.•FT-ICR MS and NMR for molecular characterization of bio-oil fractions.•Flash chromatography presents some advantages for the extensive bio-oil characterization.•Achieved fractions can be used for further upgrading process.