The target of agricultural biomass waste recovery from hydrolysis treatment is presented by comparing the performance of two different types of enzymatic polymeric membranes that were previously developed and characterized, based on a polysulfone derivative or monolithic polymers. Our aim was to achieve in one single step both enzymatic catalyzed hydrolysis of the xylan polysaccharide and the separation of the released products for the recovery of the short chain xylooligosaccharides. We present the behaviour of two different membrane modules operating in different procedure settings. The possible reuse of the membranes has also been evaluated. Xylooligosaccharides products have been characterized using Matrix Assisted Laser Desorption Ionization-Time of Flight-Mass Spectrometry (MALDI-TOF-MS). The application of such enzymatic membranes enables the recovery of short chain xylooligosaccharides from biomass waste treatment, which has many potential applications in the food and pharmaceutical industries as well in the production of renewable energy. (c) 2007 Elsevier B.V. All rights reserved.