A Stability-Indicating HPLC-DAD Method for Determination of Stiripentol: Development, Validation, Kinetics, Structure Elucidation and Application to Commercial Dosage Form

Journal of Analytical Methods in Chemistry - Tập 2014 - Trang 1-10 - 2014
Hany W. Darwish1,2, Ali S. Abdelhameed2, Mohamed I. Attia3,2, Ahmed H. Bakheit2, Nasr Y. Khalil2, Abdulrahman A. Al‐Majed2
1Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr El-Aini street, Cairo 11562, Egypt
2Department of Pharmaceutical Chemistry, College of Pharmacy, King Saud University, P. O. Box 2457, Riyadh, 11451, Saudi Arabia
3Department of Medicinal and Pharmaceutical Chemistry, Pharmaceutical and Drug Industries Research Division, National Research Centre, Dokki, Giza 12622, Egypt

Tóm tắt

A rapid, simple, sensitive, and accurate isocratic reversed-phase stability-indicating high performance liquid chromatography method has been developed and validated for the determination of stiripentol and its degradation product in its bulk form and pharmaceutical dosage form. Chromatographic separation was achieved on a Symmetry C18 column and quantification was achieved using photodiode array detector (DAD). The method was validated in accordance with the ICH requirements showing specificity, linearity (r2=0.9996, range of 1–25 μg/mL), precision (relative standard deviation lower than 2%), accuracy (mean recovery100.08±1.73), limits of detection and quantitation (LOD = 0.024 and LOQ = 0.081 μg/mL), and robustness. Stiripentol was subjected to various stress conditions and it has shown marked stability under alkaline hydrolytic stress conditions, thermal, oxidative, and photolytic conditions. Stiripentol degraded only under acidic conditions, forming a single degradation product which was well resolved from the pure drug with significantly different retention time values. This degradation product was characterized by1H-NMR and13C-NMR spectroscopy as well as ion trap mass spectrometry. The results demonstrated that the method would have a great value when applied in quality control and stability studies for stiripentol.

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Tài liệu tham khảo

2005, Pharmacological Reports, 57, 154

10.1107/S0108270188007772

10.1016/S0378-4347(01)00502-3

10.1016/0920-1211(92)90088-B

10.1016/j.tetasy.2013.02.006

1984, Pharmacokinetic properties and metabolic profile of stiripentol in primates, 199

10.1111/j.1528-1157.1983.tb04632.x

10.1111/j.1528-1167.2011.03008.x

10.1111/epi.12303

1984, Arzneimittel-Forschung, 34, 199

1978, Cellular and Molecular Biology, 23, 455

10.1111/j.1528-1167.2006.00497.x

2000

2003

2003

1998

10.1016/0920-1211(94)90001-9

2012, International Journal of Chemistry, 4, 7

1988, Journal of the Spanish Association of Hospital Pharmacists, 12, 197

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Journal of Analytical Methods in Chemistry

Tập 2014

1-10

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