Ambient ionization mass spectrometry imaging (MSI) has been increasingly used to investigate the molecular distribution of biological tissue samples. Here, we report the integration and optimization of desorption electrospray ionization (DESI) and liquid-microjunction surface sampling probe (LMJ-SSP) with a chip-based high-field asymmetric waveform ion mobility spectrometry (FAIMS) device to image metabolites, lipids, and proteins in biological tissue samples. Optimized FAIMS parameters for specific molecular classes enabled semitargeted detection of multiply charged molecular species at enhanced signal-to-noise ratios (S/N), improved visualization of spatial distributions, and, most importantly, allowed detection of species which were unseen by ambient ionization MSI alone. Under static DESI-FAIMS conditions selected for transmission of doubly charged cardiolipins (CL), for example, detection of 71 different CL species was achieved in rat brain, 23 of which were not observed by DESI alone. Diagnostic CL were imaged in a human thyroid tumor sample with reduced interference of isobaric species. LMJ-SSP-FAIMS enabled detection of 84 multiply charged protein ions in rat brain tissue, 66 of which were exclusive to this approach. Spatial visualization of proteins in substructures of rat brain, and in human ovarian cancerous, necrotic, and normal tissues was achieved. Our results indicate that integration of FAIMS with ambient ionization MS allows improved detection and imaging of selected molecular species. We show that this methodology is valuable in biomedical applications of MSI for detection of multiply charged lipids and proteins from biological tissues.
In this work, we synthesized ZnO nanorods by a wet chemical process. By varying different parameters of the synthesis process like precursor concentration, solvent used, surfactant, temperature, and reaction time, we were able to control the aspect ratio (l/d) and sharpness factor (S f ) h/b) of the rods. Rods with an aspect ratio of ∼20 and a sharpness factor of 10 were repeatedly obtained and characterized from scanning electron microscopy. High-resolution transmission electron microscopy and dark field analysis revealed that nanorods grow as a single crystal along the c axis [0001]. UV and visible emission was obtained in both flat-and sharp-terminated rods. According to the XPS analysis, rods present an excess of Zn 2+ of ∼4% that is responsible for the strong yellow emission band. Such defects were removed by annealing of the sample at 200 °C for 2 h. Possible mechanisms of changes in the morphology produced by changes in the synthesis process are also discussed.
The interactions of Pt nanoparticles, deposited by evaporation onto highly oriented pyrolytic graphite surfaces modified by kiloelectronvolt Ar+ beam treatment, have been studied by X-ray photoelectron spectroscopy core-level line shape analysis. The C1s and Pt4f7/2 peaks were each considered to be composed of one asymmetric peak, and changes in their asymmetry parameters were used to study their interfacial interactions. In addition to these changes, strong signal intensity changes with time were found for both the C1s and Pt4f peaks, indicating an initial crystalline orientational instability of the Pt nanoparticles, which is supported by time-dependent high-resolution electron microscopy studies at elevated temperatures.
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