title: Investigation of solvent-free MALDI-TOFMS sample preparation methods for the analysis of organometallic and coordination compounds.
abstract: An investigation of various solvent-free matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) sample preparation methods for the characterization of organometallic and coordination compounds is described. Such methods are desirable for insoluble materials, compounds that are only soluble in disadvantageous solvents, or complexes that dissociate in solution, all of which present a major "difficulty" to most mass spectrometry techniques. First-row transition metal acetylacetonate complexes, which have been characterized previously by solution preparation MALDI-TOFMS, were used to evaluate the various solvent-free procedures. These procedures comprise two distinct steps: the first being the efficient "solids mixing" (the mixing of sample and matrix), and the second being the effective transfer of the sample/matrix mixture to the MALDI target plate. This investigation shows that vortex mixing is the most efficient first step and that smearing using a microspatula is the most effective second step. In addition, the second step is shown to be much more critical than the first step in obtaining high-quality data. Case studies of truly insoluble materials highlight the importance of these techniques for the wider chemistry community.
authors.affiliation: EPSRC National Mass Spectrometry Service Centre (NMSSC), Institute of Mass Spectrometry (IMS), School of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP, UK.
authors.forename: Laura
authors.initials: L
authors.lastname: Hughes
authors.forename: Mark F
authors.initials: MF
authors.lastname: Wyatt
authors.forename: Bridget K
authors.initials: BK
authors.lastname: Stein
authors.forename: A Gareth
authors.initials: AG
authors.lastname: Brenton
mesh_terms: D009942:Organometallic Compounds / Q000032:analysis* / Q000302:isolation & purification; D011108:Polymers / Q000737:chemistry; D012995:Solubility; D012997:Solvents / Q000737:chemistry; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization
chemical_list: D009942:Organometallic Compounds; D011108:Polymers; D012997:Solvents