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A method is described for high-resolution label-free molecular imaging of human bone tissue. To preserve the lipid content and the heterogeneous structure of osseous tissue, 4 μm thick human bone sections were prepared via cryoembedding and tape-assisted cryosectioning, circumventing the application of organic solvents and a decalcification step. A protocol for comparative mass spectrometry imaging (MSI) on the same section was established for initial analysis with time-of-flight secondary ion mass spectrometry (TOF-SIMS) at a lateral resolution of 10 μm to <500 nm, followed by atmospheric pressure scanning microprobe matrix-assisted laser desorption/ionization (AP-SMALDI) Orbitrap MSI at a lateral resolution of 10 μm. This procedure ultimately enabled MSI of lipids, providing the lateral localization of major lipid classes such as glycero-, glycerophospho-, and sphingolipids. Additionally, the applicability of the recently emerged Orbitrap-TOF-SIMS hybrid system was exemplarily examined and compared to the before-mentioned MSI methods.
The structures and properties of silver selenide samples strongly depend on the method of preparation. Thin films prepared by pulsed laser deposition (PLD) contain lamellae of two low-temperature modifications of Ag2Se whose structures were analyzed in detail by electron microscopy techniques. Besides the stable and known Naumannite-type phase (LT1), a metastable phase was observed (LT2), and the phase transformation was examined in situ. Via cooling and annealing, LT2 becomes dominant in thin films, thus enabling solving the structure of LT2 by electron diffraction. These experiments and HRTEM point to an Acanthite-type (stable low-temperature modification of Ag2S) structure of LT2. Rapid-quenching procedures were applied for the first synthesis of LT2 as bulk sample. Depending on the conditions of melt spinning experiments, well-defined products were formed. In one series, we found a separation of LT1 and LT2 into distinct morphologies, i.e. microspheres and dendrites, respectively. The results on the magnetoresistance of the rapidly quenched materials support previous work.