Silica Monolith Nested in Sponge (SiMNS): A Composite Monolith as a New Solid Phase Extraction Material for Environmental Analysis.

We report a new material of a composite silica monolith nested in sponge (SiMNS) and demonstrate an application in the trace analysis of environmental contaminants in water. SiMNS is prepared through sponge absorption of a hydrolyzed mixture of siloxanes and in situ gel formation within the pores. Images obtained using scanning electron microscopy show that the silica and sponge skeletons are mutually nested in SiMNS. This nested composite structure of SiMNS enhances the mechanical flexibility of the material, allowing for reproducible production of desirable sizes and shapes for solid phase extraction (SPE) cartridges without the need to use frits. Functionalization of SiMNS provides appropriate SPE options for selective and efficient extraction of specific contaminants. SPE cartridges packed with functionalized SiMNS-SO3Na have high extraction capacity, good stability in the pH range of 2 to 11, and efficient enrichment of dipeptides in water. Extraction of six dipeptides from water using these new SiMNS-SO3Na SPE cartridges followed by HPLC-MS/MS analysis results in improved method detection limits (MDLs) of 0.02-1.3 ng/L and method quantification limits (MQLs) of 0.05-4.3 ng/L. Successful identification and quantification of three dipeptides, Tyr-Gly, Phe-Gly, and Tyr-Ala, from raw water demonstrates a useful application of the new SPE materials for environmental analysis of trace contaminants. On the basis of this work, a range of functionalized SiMNS materials can be produced and tailored for various environmental and exposomic analyses.