title: Structural characterization of silicone polymers using compositional ultra-high performance liquid chromatography separation, electrospray ionization, and high resolution/accurate mass.
abstract: In this article, the development of an on-line ultra-high performance liquid chromatography (UHPLC)-high resolution/accurate mass (HR/AM) methodology for timely characterization of a broad range of silicone polymers is described. Electrospray ionization was optimized for silicone polymers to enable the direct coupling of the separation with mass spectrometry. Reverse-phase UHPLC was optimized to provide a high resolution separation of oligomers by molar mass and by end-group composition. With the high resolution compositional separation, multiple pseudo-molecular ion species were indexed with retention time and assisted in rapid identification of oligomer species. Relative retention times of different oligomer end-group species separated based on polarity provided additional information to aid data interpretation. These additional pieces of information were combined with accurate mass to provide a high information content analysis in a relatively short time frame. This methodology was applied to polymer end-group characterization, as well as comparative analysis examples.
authors.affiliation: Analytical and Material Science Division, Bausch and Lomb, Inc., Rochester, NY 14609, USA. Electronic address: andrew.hoteling@bausch.com.
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Hoteling
authors.affiliation: Analytical and Material Science Division, Bausch and Lomb, Inc., Rochester, NY 14609, USA.
authors.forename: Peter T
authors.initials: PT
authors.lastname: Papagelis
keywords: Compositional separation of polymers; High resolution/accurate mass; Polymer mass spectrometry; Silicone polymer characterization; UHPLC