Get access

Design of Experiment (DoE) as a Tool for the Optimization of Source Conditions in SEC-ESI-MS of Functional Synthetic Polymers Synthesized via ATRP

Authors

  • Till Gruendling,

    1. Preparative Macromolecular Chemistry, Institut für Technische und Polymerchemie, Universität Karlsruhe (TH)/Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany
    2. Bioanalytical Mass Spectrometry Facility, UNSW Analytical Centre, The University of New South Wales, Sydney, New South Wales 2052, Australia
    Search for more papers by this author
  • Michael Guilhaus,

    1. Bioanalytical Mass Spectrometry Facility, UNSW Analytical Centre, The University of New South Wales, Sydney, New South Wales 2052, Australia
    Search for more papers by this author
  • Christopher Barner-Kowollik

    Corresponding author
    1. Preparative Macromolecular Chemistry, Institut für Technische und Polymerchemie, Universität Karlsruhe (TH)/Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany
    • Preparative Macromolecular Chemistry, Institut für Technische und Polymerchemie, Universität Karlsruhe (TH)/Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany.
    Search for more papers by this author

Abstract

Design of experiment (DoE) is applied to establish the optimum ionization conditions for analyzing synthetic polymers via coupled size exclusion chromatography electrospray ionization mass spectrometry (SEC-ESI-MS) yielding maximum ionization efficiency. The ion source conditions were optimized with regard to the ionization efficiency, the amount of fragmentation, as well as the formation of salt adducts. A D-optimal experimental design was employed for this purpose and the recorded data were evaluated by a quadratic response surface model, accounting for possible interactions between the individual source settings. It was established that the ionization efficiency can be improved by up to one order of magnitude without compromising the softness of the ionization process and that optimal ionization conditions are found at similar source settings regardless of the charge state. The present optimization exercise therefore provides a hands-on guide for the use of experimental design to determine optimum ionization conditions during the SEC-ESI-MS of functional polymers.

original image

Ancillary