The removal of contaminants from aqueous media is a challenge faced in many engineering systems. In particular, fermentation processes during biofuel production is hampered by a variety of toxic compounds present in hemicellulosic hydrolysates. Adsorption is an efficient and economic method of reduction in the amounts of phenolic compounds, acetic acid, aromatic compounds, furfural and hydroxymethylfurfural normally found in hemicellulosic hydrolysates. Activated carbon is currently the most widely used adsorbent. However, its poor reusability and its limited capacity to uptake larger molecules due to size exclusion effects necessitate the investigation into alternative materials. Carbon nanomaterials exhibit high specific surface area and open pore structure, making them very compelling for hydrolysate detoxification. To overcome the tendency of carbon nanomaterials to aggregate, which greatly reduces the number of sites available for adsorption, we developed mesoporous, nitrogen-doped, reduced graphene oxide aerogels with an open three-dimensional network. Graphene oxide was first prepared from renewable carbon sources and reduced by hydrothermal treatment to form hydrogels, which were then freeze-dried in tert-butanol to form aerogel sorbents. By adjusting the different synthesis parameters (i.e. temperature, pH, chemical dosages…), we were able to finely control the pore structure and chemical composition of the nitrogen-doped graphene aerogels, as measured by nitrogen physisorption and elemental analysis. Results revealed superior adsorption properties than activated carbon for the hydrolysate detoxification, which improved fermentation yields.