title: Application of polymer based stationary phases in high performance liquid chromatography and capillary high performance liquid chromatography hyphenated to microcoil 1H nuclear magnetic resonance spectroscopy.
abstract: The increased demand for chromatographic materials that are able to achieve a fast separation of large quantities of structure analogues is a great challenge. It is known that polymer based chromatographic materials have a higher loadability, compared to silica based sorbents. Unfortunately these polymer materials cannot be used under high pressure which is necessary in order to obtain high flow rates, and hence long times are needed to perform a separation. However, by immobilizing a polymer on a mechanically stable porous silica core, this problem can be circumvented and higher flows become feasible on these materials. Especially for capillary liquid chromatography hyphenated with nuclear magnetic resonance a high loadability is of great importance in order to obtain sharp, resolved, and concentrated peaks thus resulting in a good signal to noise ratio in the NMR experiment. Therefore, a highly shape selective chromatographic sorbent was developed by covalently immobilizing a poly(ethylene-co-acrylic) acid copolymer (-CH(2)CH(2)-)(x)[CH(2)CH(CO(2)H)-](y) (x=119, y=2.4) with a mass fraction of acrylic acid of 5% as stationary phase on silica via a spacer molecule (3-glycidoxypropyltrimethoxysilane). First, the loadability of this sorbent compared to C(30) is demonstrated by the HPLC separation of two xanthophyll isomers. Subsequently, it has been successfully employed in the hyphenation of capillary HPLC with microcoil (1)H NMR spectroscopy by separating and identifying a highly concentrated solution of the tocopherol homologues.
authors.affiliation: Institute of Organic Chemistry, University of Tuebingen, Auf der Morgenstelle 18, 72076 Tuebingen, Germany.
authors.forename: Marc David
authors.initials: MD
authors.lastname: Grynbaum
authors.forename: Christoph
authors.initials: C
authors.lastname: Meyer
authors.forename: Karsten
authors.initials: K
authors.lastname: Putzbach
authors.forename: Jens
authors.initials: J
authors.lastname: Rehbein
authors.forename: Klaus
authors.initials: K
authors.lastname: Albert
mesh_terms: D000180:Acrylic Resins / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D006859:Hydrogen; D014975:Lutein / Q000302:isolation & purification; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D011095:Polyethylenes / Q000737:chemistry; D024505:Tocopherols / Q000302:isolation & purification; D024341:Xanthophylls / Q000302:isolation & purification; D065146:Zeaxanthins
chemical_list: D000180:Acrylic Resins; D011095:Polyethylenes; D024341:Xanthophylls; D065146:Zeaxanthins; D006859:Hydrogen; C083316:(polyethylene-acrylic acid) copolymer; D024505:Tocopherols; D014975:Lutein