Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. The development of solvent-free sample preparation methods has enabled MALDI to analyze insoluble materials and, interestingly, can provide higher-quality mass spectral data. Although the utility of solvent-free sample preparation for MALDI has been demonstrated, the reasons for its success are only now being discovered. In this study, we use microscopy tools to image samples prepared using solvent-free methods to examine the morphology of these samples. The samples are prepared using a simple vortex method. Our results show that the average particle size of typical MALDI matrices is reduced from their original tens to hundreds of micrometers to hundreds of nanometers. This size reduction of the matrix occurs in one minute using the vortex method. We also observe remarkably smooth and homogeneous sample morphologies for the laser to interrogate, especially considering the relatively crude methods used to prepare our samples. © 2008 American Society for Mass Spectrometry.
Hanton, S. D., McEvoy, T. M., & Stets, J. R. (2008). Imaging the Morphology of Solvent-Free Prepared MALDI Samples. Journal of the American Society for Mass Spectrometry, 19(6), 874–881. https://doi.org/10.1016/j.jasms.2008.02.009