[Post-print] A new mass spectrometry based approach for organic synthesis monitoring
Date
2019-08-12Author
Termopoli, Veronica
Torrisi, Elena
Famiglini, Giorgio
Palma, Pierangela
Zappia, Giovanni
Cappiello, Achille
Vandergrift, Gregory W.
Zvekic, Misha
Krogh, Erik T.
Gill, Chris G.
Metadata
Show full item recordAbstract
Current mass spectrometry-based methodologies for synthetic organic reaction monitoring largely use
electrospray ionization (ESI), or other related atmospheric pressure ionization-based approaches. Monitoring of complex,
heterogeneous systems may be problematic because of sampling hardware limitations, and many relevant analytes (neutrals)
exhibit poor ESI performance. An alternative monitoring strategy addressing this significant impasse is condensed phase
membrane introduction mass spectrometry using liquid electron ionization (CP-MIMS-LEI). In CP-MIMS, a semi-permeable
silicone membrane selects hydrophobic neutral analytes, rejecting particulates and charged chemical components. Analytes
partition through the membrane, and are then transported to the LEI interface for sequential nebulization, vaporization, and
ionization. CP-MIMS and LEI are both ideal for continuous monitoring applications of hydrophobic neutral molecules. We
demonstrate quantitative reaction monitoring of harsh, complex reaction mixtures (alkaline, acidic, heterogeneous) in protic
and aprotic organic solvents. Also presented are solvent-membrane compatibility investigations, and in situ, quantitative
monitoring of catalytic oxidation and alkylation reactions.
Description
Post-printIdentifier (Other)
DOI: 10.1021/acs.analchem.9b02681DOI: 10.25316/IR-15270