In this study, the effect of a combined treatment consisting of calcium hydroxide (CH) followed by activated carbon (AC) on the purification of hemicellulose in the pre-hydrolysis liquor (PHL) from pulping process has been evaluated. The results show that lignin and furfural of PHL are efficiently removed, and the lignin removal is achieved by forming complexes onto CH particles in the CH treatment process, while acetic acid (acetate) is formed from the hydrolysis of acetyl groups present in the dissolved hemicelluloses in the PHL. The loss of xylo-oligosaccharides (XOS) is moderate, even at a high CH dosage of 0.8% while the xylose concentration is essentially unchanged. For the AC treatment, the optimal treating pH can enhance the interactions between AC and residual lignin and change the zeta potential of AC resulting in improved lignin adsorption onto AC. An increase of AC dosage has the tendency to adsorb more XOSDP>6 than XOSDP2~6. Overall, 66.9% of lignin and 70.1% of furfural removals are achieved under the optimal conditions of CH and AC treatment process, with a 5.9% total xylosugars loss. The present combination of CH and AC treatment process was more effective and selective for purification of xylosugars of PHL.