Development and validation of a stability-indicating UHPLC method for assay of felbamate and related substances

• Autorzy: Shetty S. K , Surendranath K. V , Kaja R. K. , Satish J , Jogul J , Manitripathi U
• Języki publikacji: EN

Abstrakty

EN

A new, sensitive, stability-indicating, and cost and time-effective isocratic reversed-phase UHPLC method has been developed for quantitative analysis of felbamate, an antiepileptic drug, both in the bulk drug and in pharmaceutical dosage forms. Chromatographic separation of felbamate and its two impurities was achieved on a C 18 column with a simple buffer-methanol mobile phase; the run time was 8 min. Quantification was achieved by ultraviolet detection. Resolution between the impurities was >2.0. Response was a linear function of concentration over the range 0.1–3.0 μg mL ^-1, correlation coefficient >0.999, for felbamate and the impurities. The method is capable of detecting the two impurities at levels of 0.002% (0.02 μg mL ^-1) of the test concentration of 1.0 mg mL ^-1 (1 μL injection). The same sensitivity was achieved for all the degradation products formed during stress studies in which the drug was subjected to hydrolysis, oxidation, photolysis, and thermal degradation. Substantial degradation occurred under acidic and basic conditions. The stressed test solutions were assayed against felbamate working standard and the mass balance in each case was close to 100%, indicating the method is stability-indicating. The method was validated for linearity, accuracy, precision, and robustness in accordance with ICH Guidelines.

Słowa kluczowe

EN

column liquid chromatography; ultra performance liquid chromatography; felbamate; forced degradation; validation; stability-indicating

• Wydawca: University of Silesia in Katowice ; Akademiai Kiado
• Czasopismo: Acta Chromatographica
• Rocznik: 2010
• Tom: Vol. 22, no. 2
• Strony: 161--172
• Opis fizyczny: Bibliogr. 13 poz., rys., tab.

Twórcy

autor

Shetty S. K

• Research and Development Laboratory United States Pharmacopeia-India Private Limited ICICI Knowledge Park Turkapally, Shameerpet, Hyderabad 500078 India
• Jawaharlal Technological University Department of Chemistry Kukatpally, Hyderabad 500072 India

autor

Surendranath K. V

• Research and Development Laboratory United States Pharmacopeia-India Private Limited ICICI Knowledge Park Turkapally, Shameerpet, Hyderabad 500078 India

autor

Kaja R. K.

• Research and Development Laboratory United States Pharmacopeia-India Private Limited ICICI Knowledge Park Turkapally, Shameerpet, Hyderabad 500078 India

autor

Satish J

• Research and Development Laboratory United States Pharmacopeia-India Private Limited ICICI Knowledge Park Turkapally, Shameerpet, Hyderabad 500078 India

autor

Jogul J

• St Kittel Science College Department of Chemistry Dharwad 580001 Karnataka India

autor

Manitripathi U

• SMR Chambers Startech Laboratories Private Limited Madinaguda, Hyderabad 500050 India

Bibliografia

• [1] J.M. Rho, S.D. Donevan, and M.A. Rogawski, J. Pharmacol. Exp. Ther., 280 (3), 1383–1391 (1997)
• [2] I.E. Leppik, F.E. Dreifuss, G.W. Pledger, et al., Neurology, 41 (11), 1785–1789 (1991)
• [3] O. Devinsky, R.E. Faught, B.J. Wilder, et al., Epilepsy Res., 20 (3), 241–246 (1995)
• [4] J. Hempenius, G. Hendriks, J. Hingstman, C.K. Mensink, J.H.G. Jonkman, and C.C. Lin, J. Pharm. Biomed. 12 , 1443–1451 (1994)
• [5] M. Contin, M. Balboni, E. Callegati, C. Candela, F. Albani, R. Riva, and A. Baruzzi, J. Chromatogr. A, 828 , 113–117 (2005)
• [6] K.M. Matar, J. Pharm. Biomed., 48 (3), 822–828 (2008)
• [7] P.H. Tang, J. Anal. Tox., 32 (5), 373–378 (2008)
• [8] P. Gur, A. Poklis, J. Saady, and J. Costantino, Anal. Tox., 19 (6), 499–503 (1995)
• [9] C.D. Thompson, M.T. Barthen, D.W. Hopper, T.A. Miller, M. Quigg, C. Hudspeth, G. Montouris, T.L. Macdonald, Epilepsia, 40 (6), 769–776 (1999)
• [10] ICH Stability Testing of New Drug Substances and Products Q1A (R2) International Conference on Harmonization, IFPMA, Geneva, 2003
• [11] J.T. Carstensen and C.T. Rhodes (Eds) Drug Stability Principles and Practices, 3rd edn., 2000
• [12] ICH Guidelines on Validation of Analytical procedures, Text and Methodology Q2 (R 1 ), FDA, Published in the Federal Register, 60, 1126, 1995
• [13] USP (2009) United States Pharmacopeia, 32nd edn., United States Pharmacopeial Convention, Rockville