title: Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC.
abstract: BACKGROUND
  Ciprofloxacin (CIP), moxifloxacin (MOX), norfloxacin (NOR) and ofloxacin (OFL), are the antibacterial synthetic drugs, belonging to the fluoroquinolones group. Fluoroquinolones are compounds susceptible to photodegradation process, which may lead to reduction of their antibacterial activity and to induce phototoxicity as a side effect. This paper describes a simple, sensitive UPLC-MS/MS method for the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products.
  
  
  RESULTS
  Chromatographic separations were carried out using the Acquity UPLC BEH C18 column; (2.1 × 100 mm, 1.7 μm particle size). The column was maintained at 40°C, and the following gradient was used: 0 min, 95% of eluent A and 5% of eluent B; 10 min, 0% of eluent A and 100% of eluent B, at a flow rate of 0.3 mL min(-1). Eluent A: 0.1% (v/v) formic acid in water; eluent B: 0.1% (v/v) formic acid in acetonitrile. The method was validated and all the validation parameters were in the ranges acceptable by the guidelines for analytical method validation. The photodegradation of examined fluoroquinolones in solid phase in the presence of excipients followed kinetic of the first order reaction and depended upon the type of analyzed drugs and coexisting substances. Photodegradation process of analyzed drugs was confirmed by differential scanning calorimetry. In addition, the identification of degradation products was carried out by mass spectrometry.
  
  
  CONCLUSIONS
  The developed UPLC-MS/MS method enables the determination of CIP, MOX, NOR and OFL in the presence of photodegradation products and identification of photodegradation products.
authors.affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.
authors.forename: Urszula
authors.initials: U
authors.lastname: Hubicka
authors.affiliation: Department of Medicinal Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.
authors.forename: Paweł
authors.initials: P
authors.lastname: Zmudzki
authors.affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.
authors.forename: Przemysław
authors.initials: P
authors.lastname: Talik
authors.affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.
authors.forename: Barbara
authors.initials: B
authors.lastname: Zuromska-Witek
authors.affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.
authors.forename: Jan
authors.initials: J
authors.lastname: Krzek
keywords: Ciprofloxacin; Differential scanning calorimetry; Kinetic evaluation; Moxifloxacin; Norfloxacin; Ofloxacin; Photodegradation; Tandem mass spectrometry; Ultra performance liquid chromatography
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