title: A direct comparison of the performance of ground, beaded and silica-grafted MIPs in HPLC and turbulent flow chromatography applications.
abstract: Spherical molecularly imprinted polymers (MIPs) specific to the beta-blocker propranolol have been synthesised using two different approaches and compared to traditional ground monolithic MIPs in HPLC and TFC applications. TFC is a LC technique used for rapid extraction of compounds directly from complex matrices. It can be easily coupled to HPLC and MS for automation of an extraction/analysis procedure. Spherical MIP beads were produced using a suspension polymerisation technique and silica/MIP composite beads by grafting MIP to spherical silica particles using a surface-bound initiator species. Synthesis of both beaded and silica-grafted MIPs was more practical than using the traditional grinding method and yields of spherical particles of the required size between 80 and 100% were routinely achieved. Under HPLC conditions, beaded and ground MIP materials showed a degree of chiral separation for all of the nine beta-blockers tested. The beaded MIP, however, showed much better flow properties and peak shape than the ground material. Silica-grafted MIP showed some separation in five of the drugs and a large improvement in peak shape and analysis times compared with both ground and beaded MIPs. The materials prepared were also used in extraction columns for Turbulent Flow Chromatography (TFC). Although no imprinting effect was observed under typical TFC conditions, beaded polymer materials showed promise for use as TFC extraction columns due to the good flow properties and clean extracts obtained.
authors.affiliation: Pfizer Global R&D Ramsgate Road, Sandwich, Kent, UK. robert.fairhurst@uea.ac.uk
authors.forename: Robert E
authors.initials: RE
authors.lastname: Fairhurst
authors.forename: Christophe
authors.initials: C
authors.lastname: Chassaing
authors.forename: Richard F
authors.initials: RF
authors.lastname: Venn
authors.forename: Andrew G
authors.initials: AG
authors.lastname: Mayes
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000737:chemistry* / Q000302:isolation & purification*; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D044085:Microfluidics / Q000295:instrumentation / Q000379:methods*; D008863:Microspheres; D010316:Particle Size; D011433:Propranolol / Q000737:chemistry* / Q000302:isolation & purification*; D012822:Silicon Dioxide / Q000737:chemistry*; D013499:Surface Properties
chemical_list: D000319:Adrenergic beta-Antagonists; D012822:Silicon Dioxide; D011433:Propranolol