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Xylooligosaccharides (XOS) have gained considerable attention worldwide as prebiotics due to their immune-strengthening activity and beneficial gut bacteria development and can be produced from xylan-rich resources by acid hydrolysis. The present study proved the organic acid hydrolysis to be beneficial for XOS yield. In this study, a recyclable and separable organic acid, i.e., furoic acid, was used for hydrolyzing xylan to produce XOS, and the response surface methodology design was applied to maximize the XOS yield; the results indicat