title: Molecular imprinted polymeric porous layers in open tubular capillaries for chiral separations.
abstract: A new method has been developed for the preparation of molecular imprinted polymers as porous layers in open tubular (MIP-PLOT) capillary column formats for use in chiral separations by capillary liquid chromatography. The synthesis was based on 'in-capillary' ultraviolet (UV) initiated polymerization using light emitting diodes (LEDs) in conjunction with the continuous delivery of the pre-polymerization reagents into the polymerization zone of the capillary using an automated capillary delivery device. The relationships between exposure times, UV-light intensity and polymer layer thickness have been determined, as well as the effects of reagent delivery rate and multiple LED exposures on the layer thickness for various compositions of pre-polymerization mixtures. The polymer surface morphology was investigated by scanning electron microscopy (SEM). The non-steroidal anti-inflammatory drug S-ketoprofen was used as the template for the preparation of the MIP imprinted PLOT coatings. The separation performance with the ketoprofen racemate was investigated by capillary liquid chromatography. In contrast to alternative methods, which require the use of expensive chiral selectors, the described MIP PLOT stationary phases used non-chiral polymer precursors to create enantioselective nano-cavities through molecular self-assembly processes. The described fabrication methods provide a new avenue to tailor-make chiral MIP-PLOT capillary columns for the separation of chiral compounds present in complex or racemic analyte mixtures of chemical and biological origin.
authors.affiliation: School of Chemistry, Monash University, Melbourne, Victoria, 3800, Australia.
authors.forename: Chadin
authors.initials: C
authors.lastname: Kulsing
authors.affiliation: Department of Analytical Chemistry, Palacky University in Olomouc, 17. Listopadu 12, Olomouc 77146, Czech Republic.
authors.forename: Radim
authors.initials: R
authors.lastname: Knob
authors.affiliation: School of Physical Sciences - Chemistry and ACROSS, University of Tasmania, Private Bag 75, Hobart 7001, Australia.
authors.forename: Mirek
authors.initials: M
authors.lastname: Macka
authors.affiliation: Department of Electronic Engineering, La Trobe University, Melbourne,Victoria, 3083, Australia.
authors.forename: Paul
authors.initials: P
authors.lastname: Junor
authors.affiliation: School of Chemistry, Monash University, Melbourne, Victoria, 3800, Australia.
authors.forename: Reinhard I
authors.initials: RI
authors.lastname: Boysen
authors.affiliation: School of Chemistry, Monash University, Melbourne, Victoria, 3800, Australia. Electronic address: milton.hearn@monash.edu.
authors.forename: Milton T W
authors.initials: MT
authors.lastname: Hearn
mesh_terms: D053801:Capillary Electrochromatography / Q000295:instrumentation / Q000379:methods*; D008855:Microscopy, Electron, Scanning; D054802:Molecular Imprinting / Q000295:instrumentation / Q000379:methods*; D011108:Polymers / Q000737:chemistry*; D016062:Porosity; D013237:Stereoisomerism
chemical_list: D011108:Polymers
keywords: Chiral separation; Light emitting diodes; Molecularly imprinted polymers; Photo-initiated polymerization; Porous layer open tubular capillaries