Abstract Life sciences research and other critical bioanalytical applications would strongly benefit from faster and higher efficiency sample preparation processes. Sample preparation before high resolution analytical methods, such as HPLC or LC/MS, can require effort and cost nearly equivalent to the actual sample analysis and data reduction. Often, sample preparation for proteomic, glycoproteomic or glycomic analyses require one or more solid phase extraction (SPE) steps. The goals of the proposed work are to apply a new class of SPE materials to improve SPE performance for these challenging applications. Novel assembled porous silica membrane (APSM) materials have been discovered, which have features that could be well applied to SPE devices. The proposed research and development activities could yield designed materials that reduce time and effort for conducting SPE, and result in samples that are recovered at higher concentrations than the currently popular large diameter silica particle packed SPE devices. AMT has recently developed a low cost tape casting method to produce APSM materials with uniform and controlled porosity, using processes that are amenable to optimizing the materials for application to a variety of SPE sample types. In this proposal, one intention is to refine the tape casting and sintering processes to produce substantial quantities of monodisperse ASPM, to build on this technology to produce high specific surface area ASPM, and to apply these new materials in SPE devices to a variety of sample types for performance evaluation. The overall goal is to make available very high performance SPE products, superior to materials that are currently available, for application in analysis of complex biological samples, pharmaceutical and biopharmaceutical applications, in fact in any current application that uses SPE for biological molecule analyses. The separations technology described will directly lead to useful products for which there is a significant technical and market demand.