High performance anion-exchange chromatography with pulse ampero-metric detector (HPAEC-PAD) is a reliable method to systematically determine the sugar contents in pulp and paper waste streams, including bleaching and extraction liquors. We used the same method to determine the sugar content of industrially produced pre-hydrolysis liquor (PHL) from a kraft-based dissolving pulp production process. The analysis showed that the traditional method cannot be applied for sugar analysis, and an improvement on the method was required. In fact, the presence of furfural in the PHL sample was the reason for the required modification. It was noted that the removal of furfural via evaporation could improve the reliability of the HPAEC technique for sugar assessments. If the concentration of furfural was higher than 0.045% (wt.) in the PHL, the error introduced in the sugar analysis was profound. Also, the industrially produced PHL contained more furfural than the laboratory produced PHL under the same hydrolysis conditions. Consequently, the concentration of furfural in the PHL should be taken into account for sugar analysis using the HPAEC technique.