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Hélène Pizzala1, Caroline Barrère, Michaël Mazarin

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PubMed
Summary

Solid-state NMR reveals mechano-induced reactions in solvent-free matrix-assisted laser desorption/ionization (MALDI) samples. Grinding 2,5-dihydroxybenzoic acid (2,5-DHB) with caesium fluoride (CsF) forms a salt, impacting polymer ionization efficiency.

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Area of Science:

  • Analytical Chemistry
  • Materials Science

Background:

  • Solid-state Nuclear Magnetic Resonance (NMR) is crucial for analyzing sample structures before Matrix-Assisted Laser Desorption/Ionization (MALDI).
  • Solvent-free sample preparation is increasingly important for specific analytical applications.

Purpose of the Study:

  • To investigate the structural characteristics of solvent-free MALDI samples using solid-state NMR.
  • To understand the interactions between 2,5-dihydroxybenzoic acid (2,5-DHB) matrix and caesium fluoride (CsF) under mechanical stress.
  • To correlate sample structure with MALDI mass analysis outcomes.

Main Methods:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy (13C, 133Cs, 19F).
  • Preparation of 2,5-DHB and CsF mixtures at varying molar ratios (1:1, 5:1, 10:1) without solvents.
  • Analysis of samples with and without poly(ethylene oxide) polymer analyte.

Main Results:

  • Solid-state grinding of 2,5-DHB and CsF induces mechano-reactions, forming a caesium salt, particularly in the presence of water.
  • The molecular organization of the MALDI sample is significantly altered by these mechano-induced reactions.
  • Despite unusual matrix/salt ratios, good quality mass spectra were obtained, showing reduced ionization efficiency for highly organized samples.

Conclusions:

  • Mechano-induced salt formation between 2,5-DHB and CsF impacts MALDI ionization efficiency.
  • Cation attachment in MALDI is matrix-dependent, influenced by the solid-state molecular organization.
  • Water plays a critical role in facilitating mechano-induced reactions in these solvent-free systems.