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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
Published on: August 22, 2017
Determination of binary polymorphic mixtures of fluconazole using near infrared spectroscopy and X-ray powder
E Ziémons1, H Bourichi, J Mantanus
1Laboratory of Analytical Chemistry, CIRM, Department of Pharmacy, University of Liège, Avenue de l'Hôpital 1, 4000 Liège, Belgium. eziemons@ulg.ac.be
Abstract:
The aim of the present study was to develop near infrared (NIR) and X-ray powder diffraction methods (XRPD) able to determine pure crystalline form II of fluconazole in a binary polymorphic mixtures containing forms II and III. In order to give a first performance estimation of both methods, these latters were pre-validated using accuracy profiles, a statistical approach based on β-expectation tolerance intervals. Both methods showed a good trueness, precision and accuracy and their β-expectation tolerance intervals were fully included within the acceptance limits. The comparative study was carried out using statistical analysis based on the work of Bland and Altman. A good agreement between the two methods was demonstrated indicating the interchangeability of NIR method with XRPD method.
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