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  • Molecularly imprinted solid phase extraction of fluconazole from pharmaceutical formulations.

Molecularly imprinted solid phase extraction of fluconazole from pharmaceutical formulations.

Talanta (2015-01-27)
S Manzoor, R Buffon, A V Rossi
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.

MATERIALS
Product Number
Brand
Product Description

Miconazole, European Pharmacopoeia (EP) Reference Standard
USP
Miconazole, United States Pharmacopeia (USP) Reference Standard
Fluconazole for peak identification, European Pharmacopoeia (EP) Reference Standard
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Dimethyl sulfoxide, United States Pharmacopeia (USP) Reference Standard
Tioconazole for system suitability, European Pharmacopoeia (EP) Reference Standard
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Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
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Acetonitrile, ≥99.5%, ACS reagent
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8-Octanoyloxypyrene-1,3,6-trisulfonic acid trisodium salt, suitable for fluorescence, ≥90% (HPCE)
Supelco
Acetonitrile, HPLC grade, ≥99.93%
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Dimethyl sulfoxide, SAJ first grade, ≥99.0%
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Dimethyl sulfoxide, ≥99.0%, suitable for absorption spectrum analysis
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Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles
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Methanol-12C, 99.95 atom % 12C
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Dimethyl sulfoxide, suitable for HPLC
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Acetonitrile, for residue analysis, JIS 5000
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Acetonitrile, for chromatography
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Dimethyl sulfoxide solution, 50 wt. % in H2O
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Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
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Methacrylic acid, SAJ first grade, ≥98.0%
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Acetonitrile, JIS special grade, ≥99.5%
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Acetonitrile, SAJ first grade, ≥99.0%
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Acetonitrile, ≥99.8%, for residue analysis, JIS 300
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Dimethyl sulfoxide, ≥99.5%
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Dimethyl sulfoxide, JIS special grade, ≥99.0%
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Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
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Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
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Acetonitrile, ≥99.8%, suitable for HPLC
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
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Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)