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Single-use aluminum foil-based laser desorption/ionization (LDI) target plates have been developed for mass spectrometry (MS) analysis and provide detection results comparable to those of commercial stainless steel plates while offering a convenient way to avoid the time-consuming surface cleaning process. Additionally, arrays of TiO2 nanoparticle spots are coated on the foil either by screen-printing or rotogravure-printing followed by sintering to form a mesoporous layer spot to act as an anchor for sample deposition. These TiO2 spots offer further functions to the Al foil, such as matrix-free laser desorption/ionization or specific affinity for in situ enrichment of phosphopeptides. The single-use TiO2-Al foils are cheap to produce, easy to use, and well suited for high-throughput proteomics research. They can also be of interest for protein post-translational modifications study.