The aim of this study was to investigate the ultrasound-assisted alkaline extraction process and structural properties of hemicellulose from sugarcane bagasse pith. Response surface model (RSM) was established in order to optimize the extraction conditions for the highest hemicellulose yield based on the single-factor experiments. A maximum total hemicellulose yield of 23.05% was obtained under the optimal conditions of ultrasonic treatment time of 28 min, KOH mass concentration of 3.7%, and extraction temperature of 53 °C, and it evidently increased 3.24% compared without ultrasound-assisted extraction. The obtained hemicellulose was analyzed by Fourier transform infrared (FT-IR) spectroscopy. The monosaccharide composition and average molecular weight of hemicellulose were characterized by using ion chromatography (IC) and gel permeation chromatography (GPC). The results indicated that xylose was dominant component in water-soluble hemicellulose (WH, 69.05%) and alkali-soluble hemicellulose (AH, 85.83%), respectively. Furthermore, the monosaccharides (otherwise xylose) and uronic acids contents of WH were higher than that of AH. Weight average molecular weight of WH was 29923 g/mol, lower than that of AH (74,872 g/mol). These results indicate that ultrasonic-assisted alkaline extraction is an efficient approach for the separation of hemicellulose from sugarcane bagasse pith.
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