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On‐line coupling of liquid chromatography at critical conditions with electrospray ionization tandem mass spectrometry for the characterization of a nitroxide‐mediated poly(ethylene oxide)/polystyrene block copolymer
Author(s) -
Girod Marion,
Phan Trang N. T.,
Charles Laurence
Publication year - 2008
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.3796
Subject(s) - chemistry , electrospray ionization , copolymer , oligomer , ethylene oxide , polystyrene , electrospray , mass spectrometry , nitroxide mediated radical polymerization , tandem mass spectrometry , chromatography , anionic addition polymerization , polymer chemistry , radical polymerization , organic chemistry , polymer
Coupling of liquid chromatography at critical conditions (LCCC) with on‐line mass spectrometry (MS) detection was implemented via an electrospray ionization (ESI) interface, using a mobile phase containing the cationizing agent. Critical conditions established for poly(ethylene oxide) were used to characterize a poly(ethylene oxide)/polystyrene block copolymer (PEO‐ b ‐PS) in both MS and MS/MS modes. As co‐oligomer molecules were successfully separated according to the PS block size, structural information could be reached from simplified MS spectra. The microstructure of this copolymer, synthesized by nitroxide‐mediated polymerization, could further be unambiguously characterized in LCCC/ESI‐MS/MS experiments since the PS block size could be reached by both the co‐oligomer chromatographic behavior and its MS/MS pattern. Copyright © 2008 John Wiley & Sons, Ltd.

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