Analysis of lignocellulose derived phenolic monomers by headspace solid-phase microextraction and gas chromatography

•HS-SPME/GC–MS – method established for analysis of lignin derived phenolic monomers.•HS-SPME/GC–MS – parameters optimized for 12 lignin derived phenolic monomers.•Quantitative analysis in complex aqueous solutions, e.g., lignocellulose hydrolyzates.•No extensive sample preparation, short sample han...

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Bibliographic Details
Published in:Journal of Chromatography A 2013-09, Vol.1307, p.144-157
Main Authors: Kolb, Michaela, Schieder, Doris, Faulstich, Martin, Sieber, Volker
Format: Article
Language:English
Subjects:
acetosyringone
Analytical chemistry
Applied sciences
Aqueous solutions
biomass
Chemistry
Chromatographic methods and physical methods associated with chromatography
Design engineering
Exact sciences and technology
Gas chromatographic methods
Gas chromatography
guaiacol
Headspace
headspace analysis
Lignin
Lignin and derivatives
Lignocellulose
mass spectrometry
Mathematical models
Monomers
Natural polymers
Optimization
p-coumaric acid
Phenols
Physicochemistry of polymers
quantitative analysis
screening
Solid-phase microextraction
solvents
temperature
vanillin
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Summary:•HS-SPME/GC–MS – method established for analysis of lignin derived phenolic monomers.•HS-SPME/GC–MS – parameters optimized for 12 lignin derived phenolic monomers.•Quantitative analysis in complex aqueous solutions, e.g., lignocellulose hydrolyzates.•No extensive sample preparation, short sample handling times, and high throughput.•Method especially suited for fast analysis and for screening. A headspace solid-phase microextraction method with subsequent GC–MS (HS-SPME/GC–MS) was established for the quantitative analysis of volatile lignin derived phenolic monomers in complex aqueous solutions. Extraction was done using a polyacrylate fiber. The optimization of HS-SPME – parameters was performed using a multi component model solution of six representative phenolic monomers identified in liquid hot water (LHW) supernatants of hydrothermally treated lignocellulosic biomass: p-coumaric acid, guaiacol, vanillin, acetosyringone, 4-hydroxy-3-methoxyphenylacetone, and acetophenone. Plackett–Burman design was applied for pre-evaluation and 23 central composite designs with star points for parameter optimization. LOQ (S/N>10) and LOD (S/N>3) were determined for 12 phenols yielding LOQ of
ISSN:0021-9673
DOI:10.1016/j.chroma.2013.07.094