This research involved developing a novel solid support for an enzyme attachment, focusing on synthesizing a polymer-silica hybrid monolith via in-situ sol-gel polymerization method. The fabrication of a very large surface area of the monolith was done using a cold mixture of poly(ethylene-glycol) (PEG) with tetraethyl-orthosilicate (TEOS) and acetic acid with different ratios of PEG amount and molecular weights, namely PEG-0.1, PEG-0.2, and PEG-0.3. The experiments were conducted at a very low temperature of 0 °C, followed by overnight gelification and aging. The sol then underwent calcination at 200 °C forming a hybrid monolith. The characterizations of hybrid monoliths were performed by Attenuated-Total Reflection-Fourier Transformed Infrared Spectroscopy (ATR-FTIR), Scanning Electron Microscope (SEM), and Surface Area and Porosity Analyzer using both Brunauer-Emmett-Teller (BET) and Barrett-Joyner-Halenda (BJH) methods to describe the developed monoliths. FTIR shows the presence of Si-O-Si stretching associated with the monolith network due to the polymerization process together with the presence of silanol functional group (Si-OH) that can be exploited further for covalent attachment with the enzyme. Results also showed that the optimum ratios for the hybrid polymer-silica synthesis were PEG-0.1with 10,000 M n surface area of mesoporous network recorded for 494.121 m 2 /g and pore volume of 0.265 cm 3 /g. These findings showed that the synthesized hybrid monolith on fused silica capillary will provide a vast surface area with desirable functional groups; thus, very promising for lipase immobilization support that can be used in future small-scale lipid transformation.