4.7 Article

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

Journal

MACROMOLECULAR RAPID COMMUNICATIONS
Volume 30, Issue 8, Pages 589-597

Publisher

WILEY-V C H VERLAG GMBH
DOI: 10.1002/marc.200800738

Keywords

design of experiment (DoE); ESI source optimization; ionization efficiency; poly(methyl methacrylate); radical polymerization; response surface design; reversible addition fragmentation chain transfer (RAFT); size exclusion chromatography electrospray ionization mass spectrometry (SEC-ESI-MS)

Funding

  1. Karlsruhe Institute of Technology (KIT)
  2. University of New South Wales

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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.

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