Analysis of lignocellulose derived phenolic monomers by headspace solid-phase microextraction and gas chromatography.
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 2(3) 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 <0.005-618nM and LOD of <0.005-412nM. Within-day and between-day tests (n=6) showed different results for the tested phenols. RSD ranged from 2% to 30% and recovery rates from 99% to 160% in LHW matrix. Tests on storage of LHW supernatants for several weeks indicated a considerable influence of temperature on the stability of the solutions which may even have to be taken into account for auto sampler handling. All in all the method allows a fast and solvent free analysis requiring low sample volumes making it a powerful tool for screening or high-throughput analysis of aqueous solutions of lignin derived aromatics.
Chemistry of Biogenic Resources, Technische Universität München, Schulgasse 16, 94315 Straubing, Germany.
Michaela
M
Kolb
Doris
D
Schieder
Martin
M
Faulstich
Volker
V
Sieber
D018533:Biomass; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D008031:Lignin / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D010636:Phenols / Q000032:analysis* / Q000737:chemistry / Q000378:metabolism; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052617:Solid Phase Microextraction / Q000379:methods*; D014908:Triticum / Q000737:chemistry
D010636:Phenols; C036909:lignocellulose; D008031:Lignin
Gas chromatography; Headspace; Lignin; Lignocellulose; Phenols; Solid-phase microextraction