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Determination of cellulose derived 5-hydroxymethyl-2-furfural content in lignocellulosic biomass hydrolysate by headspace gas chromatography

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Abstract

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.

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Acknowledgments

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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Authors and Affiliations

  1. College of Material Engineering, Fujian Agriculture and Forestry University, Fuzhou, 350002, China

    Hui-Chao Hu, Yu Zhang, Tong Zeng, Weining Zhou, Lihui Chen, Liulian Huang & Yonghao Ni

  2. Limerick Pulp and Paper Centre, University of New Brunswick, P.O. Box 4400, Fredericton, Canada

    Yonghao Ni

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  1. Hui-Chao Hu
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  2. Yu Zhang
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  3. Tong Zeng
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  4. Weining Zhou
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  5. Lihui Chen
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  6. Liulian Huang
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  7. Yonghao Ni
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Correspondence to Hui-Chao Hu or Lihui Chen.

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Hu, HC., Zhang, Y., Zeng, T. et al. Determination of cellulose derived 5-hydroxymethyl-2-furfural content in lignocellulosic biomass hydrolysate by headspace gas chromatography. Cellulose 25, 3843–3851 (2018). https://doi.org/10.1007/s10570-018-1857-5

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