Determination of itraconazole and its photodegradation products with kinetic evaluation by ultra-performance liquid chromatography/tandem mass spectrometry.
A simple and reproducible UPLC-MS/MS method for the determination of itraconazole (ITZ) and its photodegradation products formed during exposure to UV-A radiation was developed. Chromatographic separations were carried out using an Acquity UPLC BEH C18column (2.1 × 100 mm, 1.7 μm particle size). The column was maintained at 40°C, and eluted under gradient conditions from 100% to 50% of eluent A over 13 min, at a flow rate of 0.3 mL min-1. Eluent A was 0.1% (v/v) formic acid in water; eluent B was 0.1% (v/v) formic acid in acetonitrile. The linear regression analysis for the calibration curve showed a good linear correlation over the concentration range 0.0066-0.15 mg mL-1with determination coefficient > 0.99. The activities of some photocatalysts during degradation process of ITZ were compared. It was found that indirect photodegradation of ITZ was more effective than direct photolysis. Under our experimental conditions the photodegradation rate constant depended on the applied catalysts with catalytic activity decreasing in the following pattern: FeCl3> TiO2/FeCl3> TiO2. The kinetic analysis of the photodegradation data revealed that the degradation of the ITZ follows first-order kinetics. The photodegradation products of ITZ were identified, and their fragmentation pathways, derived from MS/MS data, were proposed. Copyright © 2016 John Wiley & Sons, Ltd.
Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688, Kraków, Poland. akryczyk@gmail.com.
Agata
A
Kryczyk
Department of Medicinal Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688, Kraków, Poland.
Paweł
P
Żmudzki
Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688, Kraków, Poland.
Urszula
U
Hubicka
D000935:Antifungal Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D017964:Itraconazole / Q000032:analysis*; D007700:Kinetics; D057230:Limit of Detection; D010782:Photolysis; D053719:Tandem Mass Spectrometry / Q000379:methods*
D000935:Antifungal Agents; D017964:Itraconazole
UPLC/MS/MS; itraconazole; kinetic evaluation; photodegradation studies