Journal
ANALYTICAL LETTERS
Volume 47, Issue 8, Pages 1334-1347Publisher
TAYLOR & FRANCIS INC
DOI: 10.1080/00032719.2013.867503
Keywords
Chemometrics; Experimental design; Fluconazole; Impurities; Liquid chromatography
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Funding
- Ministry of Education, Science, and Technological Development of the Republic of Serbia [172052]
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This paper presents the development and optimization of a liquid chromatographic method for the determination of fluconazole and its impurities by experimental design methodology. Four experimental design types were applied: two-level full factorial design, central composite design, Box-Behnken design, and three-level full factorial design. The advantages and drawbacks of each design are described and detailed statistical evaluation of mathematical models was performed. The central composite design and three-level full factorial design created significantly better models comparing to the other methods. As the central composite design requires a smaller number of experiments, its models were used for theoretical examination of experimental space. Multiobjective optimization aiming to achieve maximal separation of all investigated substances and minimal analysis duration was performed by a grid point search. The defined optimal separation was achieved on a C-18 (125mmx4mm, 5 mu m particle size) column with a mobile phase consisting of acetonitrile and water (5mM ammonium formate) (15:85, v/v); a column temperature of 25 degrees C; a flow rate of 1.2mLmin(-1); and a detection wavelength of 260nm.
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