A validated stability-indicating isocratic LC method for levofloxacin in the presence of degradation products and its process-related impurities

Czasopismo : Acta Chromatographica
Tytuł artykułu : A validated stability-indicating isocratic LC method for levofloxacin in the presence of degradation products and its process-related impurities

Autorzy :
Sajewicz, M.
University of Silesia Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland,
Gontarska, M.
University of Silesia Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland,
Kronenbach, D.
University of Silesia Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland,
Berry, E.
University of Silesia Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland,
Kowalska, T.
University of Silesia Institute of Chemistry 9 Szkolna Street 40-006 Katowice Poland, teresa.kowalska@us.edu.pl,
Deshpande, P. B.
A.I.S.S.M.S. College of Pharmacy Department of Pharmaceutical Analysis Kennedy Road Pune 411001 MH India, padmanabh77@yahoo.co.in,
Gandhi, S. V.
A.I.S.S.M.S. College of Pharmacy Department of Pharmaceutical Analysis Kennedy Road Pune 411001 MH India,
Gaikwad, N. V.
A.I.S.S.M.S. College of Pharmacy Department of Pharmaceutical Analysis Kennedy Road Pune 411001 MH India,
Khandagle, K. S.
A.I.S.S.M.S. College of Pharmacy Department of Pharmaceutical Analysis Kennedy Road Pune 411001 MH India,
Sateesh, J. N.
PRRM College of Pharmacy Department of Chemistry Kadapa Andhra Pradesh India, nagasateesh@gmail.com,
Subba Reedy, G. V.
JNTUA College of Engineering Department of Chemistry Pulivendula, Y.S.R (Kadapa) Andhra Pradesh India,
Jayaveera, K. N.
awaharlal Nehru Technological University Anantapur Oil Technology Research Institute Anantapur Andhra Pradesh India,
Dhayalamurthi, S.
Mother Theresa Post Graduate & Research Institute of Health Sciences Department of Chemistry, College of Pharmacy Gorimedu Puducherry India,
Abstrakty : The objective of the current study is to develop a validated specific stability-indicating isocratic reversed-phase liquid chromatographic method for the quantitative determination of levofloxacin and its related substances in pharmaceutical dosage forms in the presence of degradation products and its process-related impurities. Forced degradation studies were performed on levofloxacin as per the International Conference on Harmonisation (ICH)-prescribed stress conditions using acid, base, oxidative, water hydrolysis, thermal stress and photolytic degradation to show the stability-indicating power of the method. Significant degradation was observed during oxidative stress; minor degradation was observed in acidic stress and no degradation was observed in other stress conditions. The chromatographic method was optimized using the samples generated from forced degradation studies and the spiked impurity solution. The analysis was carried out with a 50 mm length × 4.6 mm i.d., 3.0 μm particle size YMC Pack Pro-C18 column using the mobile phase consisting of a mixture of 1.0% (v/v) triethylamine in water with pH adjusted to 6.30, using orthophosphoric acid, methanol and acetonitrile (7.7:1.3:1.0) pumped at a flow rate of 0.8 mL min−1 with ultraviolet (UV) detection at 235 nm. The limit of detection and the limit of quantification for the levofloxacin and its process-related impurities were established. The stressed test solutions were assayed against the qualified working standard of levofloxacin and the mass balance in each case was in between 99.1% and 99.9%, indicating that the developed liquid chromatography (LC) method was a stability-indicating technique. Validation of the developed LC method was carried out as per ICH requirements.

Słowa kluczowe : levofloxacin, isocratic reversed-phase liquid chromatography, forced degradation, validation, stability indicating,
Wydawnictwo : University of Silesia in Katowice
Rocznik : 2012
Numer : Vol. 24, no. 1
Strony : 23 – 36
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DOI :
Cytuj : Sajewicz, M. ,Gontarska, M. ,Kronenbach, D. ,Berry, E. ,Kowalska, T. ,Deshpande, P. B. ,Gandhi, S. V. ,Gaikwad, N. V. ,Khandagle, K. S. ,Sateesh, J. N. ,Subba Reedy, G. V. ,Jayaveera, K. N. ,Dhayalamurthi, S. , A validated stability-indicating isocratic LC method for levofloxacin in the presence of degradation products and its process-related impurities. Acta Chromatographica Vol. 24, no. 1/2012
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