title: Synthesis by precipitation polymerisation of molecularly imprinted polymer microspheres for the selective extraction of carbamazepine and oxcarbazepine from human urine.
abstract: Two molecularly imprinted polymers (MIPs), in the physical form of well-defined polymer microspheres, were synthesised via precipitation polymerisation (PP) using an antiepileptic drug, carbamazepine (CBZ), as template molecule, methacrylic acid as functional monomer and either divinylbenzene 80 (DVB-80) or a mixture of DVB-80 and ethylene glycol dimethacrylate (EGDMA) as crosslinking agents. The MIP obtained using DVB-80 alone as crosslinking agent (MIP A) had a narrow particle size distribution (9.5+/-0.5 microm) and a well-developed permanent pore structure (specific surface area in the dry state=758 m(2)g(-1)), whereas when a mixture of DVB-80 and EGDMA (MIP B) were used as crosslinking agents, the polymer obtained had a broader particle size distribution (6.4+/-1.8 microm) and a relatively low specific surface area (23 m(2)g(-1)). The molecular recognition character of both polymers was evaluated by means of LC and then a molecularly imprinted solid-phase extraction (MISPE) protocol; CBZ was recognised by both polymers, and useful cross-selectivity for oxcarbazepine (OCBZ), which is the main metabolite of CBZ, also observed. In a detailed bioanalytical study, MIP A was selected in preference to MIP B since MIP A enabled a high volume of sample to be extracted such that lower limits of detection were achievable using this polymer. High recoveries of CBZ and OCBZ were obtained in a MISPE protocol when 50 m L of human urine spiked at 0.2 mg L(-1) were percolated through MIP A (90% and 83%, respectively).
authors.affiliation: Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Tarragona, Spain.
authors.forename: A
authors.initials: A
authors.lastname: Beltran
authors.forename: R M
authors.initials: RM
authors.lastname: Marcé
authors.forename: P A G
authors.initials: PA
authors.lastname: Cormack
authors.forename: F
authors.initials: F
authors.lastname: Borrull
mesh_terms: D002220:Carbamazepine / Q000031:analogs & derivatives* / Q000652:urine*; D011232:Chemical Precipitation; D002853:Chromatography, Liquid; D006801:Humans; D006863:Hydrogen-Ion Concentration; D008855:Microscopy, Electron, Scanning; D008863:Microspheres; D054802:Molecular Imprinting / Q000379:methods*; D000078330:Oxcarbazepine; D011108:Polymers / Q000138:chemical synthesis*; D016062:Porosity; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction
chemical_list: D011108:Polymers; D002220:Carbamazepine; D000078330:Oxcarbazepine