The combination of planar chromatography with desorption/ionization mass-spectrometry (MS) techniques provides chemists with unique tools for fast and simple separation of mixtures followed by the detection of analytes by the most powerful analytical method. Since its introduction in the early 1990s, thin-layer chromatography (TLC)/matrix-assisted mass spectrometry (MALDI) has been used for the analysis of a wide range of analytes, including natural and synthetic organic compounds. Nowadays, new desorption/ionization approaches have been developed and applied in conjunction with planar chromatography competing with MALDI. This review covers recent developments in the combination of TLC with various desorption/ionization MS methods which were made in recent several years.

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This review is focused on planar chromatography hyphenated with mass-spectrometric detection for analysis of low-molecular-mass solutes. Various kinds of hyphenations are discussed with attention paid to the preparation of thin layer plates suited both for the mass-spectrometric detection of the resolved solutes direct from thin-layer plates and for indirect mass-spectrometric detection of the resolved solutes, performed by scraping, extracting, purifying, and concentrating the analyte from the thin-layer chromatography plate. Plates with monolithic layers are relatively new for thin-layer chromatography but they can successfully be combined with mass-spectrometric technique in a pursuit of comprehensive local sample composition information. Preparation of monolithic layers of different porosity and structure based on organic, inorganic, and composite materials is illustrated together with examples of successful separation and detection of low-molecular-mass solutes by means of matrix-assisted and surface-assisted laser desorption mass spectrometry.