The possibilities of an integration of matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) as an high-throughput screening tool into the workflow of combinatorial materials research are discussed. A multiple layer sample preparation technique for MALDI is described in detail and its possibilities of automation and miniaturization are discussed. Automated MALDI sample preparation could be performed within an automated synthesizer robot as well as with an ink-jet printer. The first approach offers the possibility of online reaction monitoring, whereas the second approach gives the opportunity of applications in ultra-high-throughput environments. Moreover, an example of high-throughput screening of a polymerization reaction by MALDI-TOFMS is discussed.

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