This study evaluated the performance of tangential flow filtration (TFF) using polymeric/cellulose cassettes and ceramic membranes for biomolecule separation. Small-scale TFF cassette and ceramic membrane systems were designed and implemented to assess membrane flux and separation efficiency using various polyethylene glycol (PEG) solutions. Comprehensive flux testing protocols were developed to establish optimal filtration conditions, which were then applied for sample generation. PEG samples with molecular weights of 200, 2000, 6000, and 20000 were used to determine molecular weight cut-off values and assess the separation efficiency of each membrane type. An analytical method based on size exclusion chromatography was developed to quantify membrane performance and provide a detailed comparison of advantages and limitations. Key evaluation factors included durability, separation efficiency, processing time, solvent compatibility, and system requirements, all of which are critical in pharmaceutical membrane selection. The findings highlight several advantages of ceramic membranes, demonstrating their potential as a viable alternative to traditional TFF cassettes for improving efficiency in pharmaceutical separations.