title: Molecularly imprinted solid phase extraction of fluconazole from pharmaceutical formulations.
abstract: This work encompasses a direct and coherent strategy to synthesise a molecularly imprinted polymer (MIP) capable of extracting fluconazole from its sample. The MIP was successfully prepared from methacrylic acid (functional monomer), ethyleneglycoldimethacrylate (crosslinker) and acetonitrile (porogenic solvent) in the presence of fluconazole as the template molecule through a non-covalent approach. The non-imprinted polymer (NIP) was prepared following the same synthetic scheme, but in the absence of the template. The data obtained from scanning electronic microscopy, infrared spectroscopy, thermogravimetric and nitrogen Brunauer-Emmett-Teller plot helped to elucidate the structural as well as the morphological characteristics of the MIP and NIP. The application of MIP as a sorbent was demonstrated by packing it in solid phase extraction cartridges to extract fluconazole from commercial capsule samples through an offline analytical procedure. The quantification of fluconazole was accomplished through UPLC-MS, which resulted in LOD≤1.63×10(-10) mM. Furthermore, a high percentage recovery of 91±10% (n=9) was obtained. The ability of the MIP for selective recognition of fluconazole was evaluated by comparison with the structural analogues, miconazole, tioconazole and secnidazole, resulting in percentage recoveries of 51, 35 and 32%, respectively.
authors.affiliation: Institute of Chemistry, University of Campinas, CP 6154, CEP 13083-970 Campinas, Brazil.
authors.forename: S
authors.initials: S
authors.lastname: Manzoor
authors.affiliation: Institute of Chemistry, University of Campinas, CP 6154, CEP 13083-970 Campinas, Brazil.
authors.forename: R
authors.initials: R
authors.lastname: Buffon
authors.affiliation: Institute of Chemistry, University of Campinas, CP 6154, CEP 13083-970 Campinas, Brazil. Electronic address: adriana@iqm.unicamp.br.
authors.forename: A V
authors.initials: AV
authors.lastname: Rossi
mesh_terms: D000097:Acetonitriles / Q000737:chemistry; D015725:Fluconazole / Q000032:analysis* / Q000737:chemistry; D007093:Imidazoles / Q000032:analysis / Q000737:chemistry; D008689:Methacrylates / Q000737:chemistry; D008795:Metronidazole / Q000031:analogs & derivatives / Q000032:analysis / Q000737:chemistry; D008825:Miconazole / Q000032:analysis / Q000737:chemistry; D054802:Molecular Imprinting; D011108:Polymers / Q000737:chemistry*; D052616:Solid Phase Extraction
chemical_list: D000097:Acetonitriles; D007093:Imidazoles; D008689:Methacrylates; D011108:Polymers; D008795:Metronidazole; C008384:methacrylic acid; C004919:ethylene dimethacrylate; D008825:Miconazole; D015725:Fluconazole; C016724:secnidazole; C020527:tioconazole; C032159:acetonitrile
keywords: Fluconazole; MIP; Molecularly imprinted polymer