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Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC.

Hubicka U, Zmudzki P, Talik P, Zuromska-Witek B, Krzek J - Chem Cent J (2013)

Bottom Line: Fluoroquinolones are compounds susceptible to photodegradation process, which may lead to reduction of their antibacterial activity and to induce phototoxicity as a side effect.Photodegradation process of analyzed drugs was confirmed by differential scanning calorimetry.In addition, the identification of degradation products was carried out by mass spectrometry.

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Affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.

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.

Conclusion: 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.

No MeSH data available.


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UPLC chromatograms registered for fluoroquinolones after photodegradation in solid phase in the presence of excipients: A – CIP RT = 2.53, B – MOX RT = 3.26, C – NOR RT = 2.45, D – OFL RT = 2.50.
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Figure 1: UPLC chromatograms registered for fluoroquinolones after photodegradation in solid phase in the presence of excipients: A – CIP RT = 2.53, B – MOX RT = 3.26, C – NOR RT = 2.45, D – OFL RT = 2.50.

Mentions: The developed UPLC method was specific to examine fluoroquinolones and guaranteed obtaining well shaped peaks both for active substances and coexisting photodegradation products. Peaks of main components were quite well resolved from photodegradation products in chromatograms and no interference that could have an influence on the obtained results was possible (Table 1). The main peak purity was examined with MS spectra using CODA algorithm (Waters Corporation, Milford, MA, USA). The investigated MS spectra uniquely contained signals corresponding to the examined fluoroquinolones and solvent. Satisfactory resolution was also obtained for photodegradation products, peaks appearing in chromatograms were sufficiently well resolved and could be analyzed by mass spectrometry (Figure 1).


Photodegradation assessment of ciprofloxacin, moxifloxacin, norfloxacin and ofloxacin in the presence of excipients from tablets by UPLC-MS/MS and DSC.

Hubicka U, Zmudzki P, Talik P, Zuromska-Witek B, Krzek J - Chem Cent J (2013)

UPLC chromatograms registered for fluoroquinolones after photodegradation in solid phase in the presence of excipients: A – CIP RT = 2.53, B – MOX RT = 3.26, C – NOR RT = 2.45, D – OFL RT = 2.50.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3750423&req=5

Figure 1: UPLC chromatograms registered for fluoroquinolones after photodegradation in solid phase in the presence of excipients: A – CIP RT = 2.53, B – MOX RT = 3.26, C – NOR RT = 2.45, D – OFL RT = 2.50.
Mentions: The developed UPLC method was specific to examine fluoroquinolones and guaranteed obtaining well shaped peaks both for active substances and coexisting photodegradation products. Peaks of main components were quite well resolved from photodegradation products in chromatograms and no interference that could have an influence on the obtained results was possible (Table 1). The main peak purity was examined with MS spectra using CODA algorithm (Waters Corporation, Milford, MA, USA). The investigated MS spectra uniquely contained signals corresponding to the examined fluoroquinolones and solvent. Satisfactory resolution was also obtained for photodegradation products, peaks appearing in chromatograms were sufficiently well resolved and could be analyzed by mass spectrometry (Figure 1).

Bottom Line: Fluoroquinolones are compounds susceptible to photodegradation process, which may lead to reduction of their antibacterial activity and to induce phototoxicity as a side effect.Photodegradation process of analyzed drugs was confirmed by differential scanning calorimetry.In addition, the identification of degradation products was carried out by mass spectrometry.

View Article: PubMed Central - HTML - PubMed

Affiliation: Department of Inorganic and Analytical Chemistry, Jagiellonian University Medical College, Faculty of Pharmacy, 9 Medyczna Street, 30-688 Kraków, Poland.

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.

Conclusion: 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.

No MeSH data available.


Related in: MedlinePlus