ABSTRACT
A specific, stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the estimation of perindopril erbumine (PDE) in tablet dosage form. The HPLC method showed adequate separation of PDE from its degradation products. The separation was achieved on a Phenomenex Luna C18 column (250 × 4.6 mm × 5 µm) using a mobile phase composition of 0.2% trifluoroacetic acid buffer and acetonitrile in the ratio of 60:40 (pH adjusted to 3 with ammonia) at a flow rate of 1 mL/min. The injection volume was 20 µL and the wavelength of detection was kept at 215 nm. Stress studies were performed with 1 mg/mL of each drug, starting with mild conditions and followed by stronger conditions to achieve sufficient degradation at approximately 5-20%. The linearity of the proposed method was investigated in the range of 2.5 to 50 µg/mL for PDE. The limits of detection and quantification were found to be 0.75 and 2.3 µg/mL, respectively.
Subject(s)
Chromatography, High Pressure Liquid/methods , Chromatography, Reverse-Phase/methods , Perindopril/analysis , Limit of Detection , Linear Models , Perindopril/chemistry , Reproducibility of Results , Tablets/chemistryABSTRACT
A validated stability-indicating RP-HPLC method for etofenamate (ETF) was developed by separating its degradation products on a C18 (250 mm × 4.6 mm 5 µm) Qualisil BDS column using a phosphate buffer (pH-adjusted to 6.0 with orthophosphoric acid) and methanol in the ratio of 20:80 % v/v as the mobile phase at a flow rate of 1.0 mL/min. The column effluents were monitored by a photodiode array detector set at 286 nm. The method was validated in terms of specificity, linearity, accuracy, precision, detection limit, quantification limit, and robustness. Forced degradation of etofenamate was carried out under acidic, basic, thermal, photo, and peroxide conditions and the major degradation products of acidic and basic degradation were isolated and characterized by (1)H-NMR, (13)C-NMR, and mass spectral studies. The mass balance of the method varied between 92-99%.
