title: A strategy for the systematic development of a liquid chromatographic mass spectrometric screening method for polymer electrolyte membrane degradation products using isocratic and gradient phase optimized liquid chromatography.
abstract: Within the scope of research for target and non-target LC-MS/MS analysis of membrane degradation products of polymer electrolyte membrane fuel cells, a systematic method development for the separation of structurally similar compounds was performed by phase optimized liquid chromatography. Five different stationary phases with different selectivities were used. Isocratic separation for 4-hydroxybenzoic acid, isophthalic acid, terephthalic acid, 4-hydroxybenzaldehyde and 4-formylbenzoic acid was achieved on a C18 and a Phenyl phase. Using the PRISMA model the separation efficiency was optimized. This was achieved on a serially connected mixed stationary phase composed of 30 mm C18, 150 mm Phenyl and 60 mm C30. For the LC-MS screening of unknown degradation products from polymer electrolyte membranes in the product water of a fuel cell, a solvent gradient is mandatory for less polar or later eluting compounds. By means of 4-mercaptobenzoic acid it could be shown that a solvent gradient can be applied in order to elute later eluting compounds in a short time. The adaptability of this method for the qualitative analysis by target and non-target LC-MS/MS screening has been shown by means of 4-hydroxybenzoic acid. The combination of solvent gradient and isocratic conditions makes this approach attractive for the purpose of a screening method for known and unknown analytes in a water sample.
authors.affiliation: Institut für Energie- und Umwelttechnik e.V., IUTA (Institute of Energy and Environmental Technology), Bliersheimer Str. 60, D-47229 Duisburg, Germany.
authors.forename: M
authors.initials: M
authors.lastname: Zedda
authors.forename: J
authors.initials: J
authors.lastname: Tuerk
authors.forename: T
authors.initials: T
authors.lastname: Teutenberg
authors.forename: S
authors.initials: S
authors.lastname: Peil
authors.forename: T C
authors.initials: TC
authors.lastname: Schmidt
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004573:Electrolytes / Q000032:analysis*; D006841:Hydrocarbons, Aromatic / Q000032:analysis / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods*; D008567:Membranes, Artificial; D011108:Polymers / Q000032:analysis*; D013997:Time Factors; D014867:Water / Q000737:chemistry
chemical_list: D004573:Electrolytes; D006841:Hydrocarbons, Aromatic; D008567:Membranes, Artificial; D011108:Polymers; D014867:Water