Stability Indicating Chromatographic methods for the Determination of Tiemonium methylsulphate

Two precise, accurate and sensitive high-performance liquid chromatographic and thin-layer chromatographic methods were developed and validated for the determination of Tiemonium methylsulphate in presence of its degradation product. Forced degradation study was performed using 2N H2SO4 on cold. Separation of the drug from its degradation product by HPLC was achieved using a X- Bridge C18 column and acetonitrile: methanol: 0.05M potassium dihydrogen phosphate in a ratio of (20: 5: 80 by volume) as a mobile phase, pH was adjusted to 3.0 ± 0.1 with ortho-phosphoric acid. The flow rate was 1.5 ml/min. Detection was performed at 235 nm. The linearity range was 2.0 to 20.0 µg/mL .The mean percentage recovery was 100.25 ± 0.660 %. The TLC method was used for separation of the drug from its degradation product using silica gel 60 F254 plates; the optimized mobile phase was water: methanol: glacial acetic acid (8: 4: 0.2 by volume). Quantitatively, the spots were scanned densitometrically at 235 nm. The linearity range was 0.5 to 10.0 µg/spot. The mean percentage recovery was 100.31 ± 0.655 %. Statistical comparison between the results obtained by these methods and those obtained by the manufacturer\'s method was done, and no significance difference was obtained.