ac9b02681_si_001.pdf (312.86 kB)
Mass Spectrometry Based Approach for Organic Synthesis Monitoring
journal contribution
posted on 2019-08-23, 19:13 authored by Veronica Termopoli, Elena Torrisi, Giorgio Famiglini, Pierangela Palma, Giovanni Zappia, Achille Cappiello, Gregory W. Vandergrift, Misha Zvekic, Erik T. Krogh, Chris G. GillCurrent 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 semipermeable 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.
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solvent-membrane compatibility investigationspressure ionization-based approachesreaction monitoringmass spectrometry-based methodologiesphase membrane introduction mass spectrometryOrganic Synthesis Monitoringsemipermeable silicone membranealternative monitoring strategyCP-MIMS-LEIsampling hardware limitationsuse electrospray ionizationESICP-MIMSLEIanalyte
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