Determination of cellulose derived 5-hydroxymethyl-2-furfural content in lignocellulosic biomass hydrolysate by headspace gas chromatography
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This paper reports a robust method for rapid determination of cellulose derived 5-hydroxymethyl-2-furfural (5-HMF) in biomass hydrolysate suspension based on headspace gas chromatography (HS-GC). The headspace equilibration at 150 °C for longer than 4 min with a pH range of 2.0–3.5 and a 50% (v/v) of ethanol content can obtain the full evaporation of 5-HMF, and eliminate the formation of additional 5-HMF generation from hexose. The linear GC response of 5-HMF was achieved by controlling the sample size within 20 μL. The results showed that this method has a good precision (relative standard deviation < 6.97%) and accuracy (recoveries ranged from 94.0 to 104.8%). The limit of quantification of the method was 51 mg/L. It was also found that a considerable amount of furfural (13.8%) and 5-HMF (18.7%) was adsorbed on condensed lignin and humins in residual biomass, and the washing procedure with ethanol can completely extract the adsorbed furfural and 5-HMF. The present method is accurate, simple, and robust, it will be a powerful tool for determining the content of 5-HMF in the liquid samples from biorefinery related processes.
Keywords5-Hydroxymethyl-2-furfural Adsorption of furfural and 5-HMF Condensed lignin and humins Ethanol assisted extraction Headspace gas chromatography
The authors acknowledge the National Natural Science Foundation of China (31700507 and 21576105), Fujian Provincial Department of Science and Technology (2015J05018), and National Key Research and Development Program of China (2017YFB0307900) for sponsoring this research.
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