Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines
| Autor: | Osama Ibrahim Abd El-Sattar, Maya S. Eissa |
|---|---|
| Rok vydání: | 2016 |
| Předmět: |
030226 pharmacology & pharmacy
01 natural sciences High-performance liquid chromatography Analytical Chemistry 03 medical and health sciences chemistry.chemical_compound Acetic acid Hydrolysis 0302 clinical medicine Limit of Detection medicine Chromatography High Pressure Liquid Detection limit Chromatography Phenylpropionates Silica gel 010401 analytical chemistry Reproducibility of Results General Medicine Loxoprofen Thin-layer chromatography 0104 chemical sciences chemistry Forced degradation Linear Models Chromatography Thin Layer Propionates Densitometry Tablets medicine.drug |
| Zdroj: | Journal of Chromatographic Science. |
| ISSN: | 1945-239X 0021-9665 |
| DOI: | 10.1093/chromsci/bmw196 |
| Popis: | Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. |
| Databáze: | OpenAIRE |
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