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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

Supelco
Methanol, analytical standard
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
Fluconazole, ≥98% (HPLC), powder
Supelco
Fluconazole, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Fluconazole, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Methanol, purification grade, 99.8%
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Tioconazole, 97%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
USP
Tioconazole, United States Pharmacopeia (USP) Reference Standard
Supelco
Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Fluconazole, European Pharmacopoeia (EP) Reference Standard
Supelco
Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
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Methanol solution, contains 0.50 % (v/v) triethylamine
Supelco
Dimethyl sulfoxide, for inorganic trace analysis, ≥99.99995% (metals basis)
Sigma-Aldrich
Methanol solution, suitable for NMR (reference standard), 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Miconazole, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Dimethyl sulfoxide, Vetec, reagent grade, 99%