title: Fast analysis of glibenclamide and its impurities: quality by design framework in capillary electrophoresis method development.
abstract: A fast capillary zone electrophoresis method for the simultaneous analysis of glibenclamide and its impurities (I(A) and I(B)) in pharmaceutical dosage forms was fully developed within a quality by design framework. Critical quality attributes were represented by I(A) peak efficiency, critical resolution between glibenclamide and I(B), and analysis time. Experimental design was efficiently used for rapid and systematic method optimization. A 3(5)//16 symmetric screening matrix was chosen for investigation of the five selected critical process parameters throughout the knowledge space, and the results obtained were the basis for the planning of the subsequent response surface study. A Box-Behnken design for three factors allowed the contour plots to be drawn and the design space to be identified by introduction of the concept of probability. The design space corresponded to the multidimensional region where all the critical quality attributes reached the desired values with a degree of probability π ≥ 90%. Under the selected working conditions, the full separation of the analytes was obtained in less than 2 min. A full factorial design simultaneously allowed the design space to be validated and method robustness to be tested. A control strategy was finally implemented by means of a system suitability test. The method was fully validated and was applied to real samples of glibenclamide tablets.
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy. sandra.furlanetto@unifi.it.
authors: Sandra
authors: S
authors: Furlanetto
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy. serena.orlandini@unifi.it.
authors: Serena
authors: S
authors: Orlandini
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy.
authors: Benedetta
authors: B
authors: Pasquini
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy.
authors: Claudia
authors: C
authors: Caprini
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy.
authors: Paola
authors: P
authors: Mura
authors: Department of Chemistry "U. Schiff", University of Florence, Via U. Schiff 6, 50019, Sesto Fiorentino, FI, Italy.
authors: Sergio
authors: S
authors: Pinzauti
mesh_terms: D004340:Drug Contamination; D019075:Electrophoresis, Capillary / Q000191:economics / Q000379:methods*; D005905:Glyburide / Q000737:chemistry*; D007004:Hypoglycemic Agents / Q000737:chemistry*; D013607:Tablets; D013997:Time Factors
chemical_list: D007004:Hypoglycemic Agents; D013607:Tablets; D005905:Glyburide
keywords: Capillary electrophoresis; Design of experiments; Design space; Glibenclamide; Impurities; Quality by design