We propose a one-stage hydrothermal extraction of sugar beet pulp leading to effective co-production of pectin and neutral monosaccharides with a relatively high yield and satisfactory purity without the presence of an acidic catalyst. The optimal experimental design methodology was used for modelling and optimizing the yield of pectin and neutral monosaccharides. In good agreement with experimental results (R2 = 0.955), the model predicts an optimal yield of pectin (approx. 121.1 g kg−1 ± 0.47 g kg−1) at a temperature and time of about 118.1 °C and 21.5 min, respectively. The highest yield of the sum of neutral monosaccharides (approx. 82.6 g kg−1 ± 0.72 g kg−1) was obtained at about 116.2 °C and 26.4 min (R2 = 0.976). The obtained results are suitable for industrial upscaling and may provide an incentive to implement a new, environmentally friendly, simple, and effective method for treating waste product from the sugar refining industry, which has proved onerous until now.
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