title: Determination of binary polymorphic mixtures of fluconazole using near infrared spectroscopy and X-ray powder diffraction: a comparative study based on the pre-validation stage results.
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.
authors.affiliation: Laboratory of Analytical Chemistry, CIRM, Department of Pharmacy, University of Liège, Avenue de l'Hôpital 1, 4000 Liège, Belgium. eziemons@ulg.ac.be
authors.forename: E
authors.initials: E
authors.lastname: Ziémons
authors.forename: H
authors.initials: H
authors.lastname: Bourichi
authors.forename: J
authors.initials: J
authors.lastname: Mantanus
authors.forename: E
authors.initials: E
authors.lastname: Rozet
authors.forename: P
authors.initials: P
authors.lastname: Lebrun
authors.forename: E
authors.initials: E
authors.lastname: Essassi
authors.forename: Y
authors.initials: Y
authors.lastname: Cherrah
authors.forename: A
authors.initials: A
authors.lastname: Bouklouze
authors.forename: Ph
authors.initials: P
authors.lastname: Hubert
mesh_terms: D002138:Calibration; D002623:Chemistry Techniques, Analytical; D002626:Chemistry, Pharmaceutical / Q000379:methods*; D003460:Crystallization; D015725:Fluconazole / Q000032:analysis*; D008956:Models, Chemical; D015233:Models, Statistical; D011208:Powders; D012044:Regression Analysis; D015203:Reproducibility of Results; D019265:Spectroscopy, Near-Infrared / Q000379:methods*; D013678:Technology, Pharmaceutical / Q000379:methods; D014961:X-Ray Diffraction / Q000379:methods*
chemical_list: D011208:Powders; D015725:Fluconazole