Validated Stability-Indicating Liquid Chromatographic Method for the Determination of Raloxifene (Anti-Osteoporotic Agent) in Tablets

Abstract

Raloxifene hydrochloride is a new anti-osteoporotic agent, effective in the treatment of breast cancer. A stability-indicating high-performance liquid chromatographic method was developed and validated for the determination of Raloxifene Hydrochloride in tablet dosage forms. Reversed-phase chromatography was performed on Shimadzu M odel LC-20AD Prominence with SPD M 20A Diode array detector using a Phenomenex Lichrosphere 100 C-18 (250 mm × 4.6 mm i.d., 5 µm particle size) column with sodium acetate: methanol (40:60, V/V) as mobile phase with a flow rate of 1 ml/min. UV detection was performed at 287 nm. Linearity was observed in the concentration range of 1.0-250 μg/mL with regression equation y = 95604 x-26215 with correlation coefficient of 0.9999. The LOD and LOQ were found to be 0.267 μg/mL and 0.813 μg/mL respectively. The percentage relative standard deviation in precision and accuracy studies was found to be less than 2%. Raloxifene hydrochloride was subjected to stress conditions of degradation in aqueous solutions including acidic, alkaline, oxidation and photolysis. It was found that the drug is highly resistant towards all degradations as the decomposition was less than 3.5%. The developed method was validated with regard to linearity, accuracy, precision, selectivity and robustness and the method was found to be precise, accurate, linear and specific.

Quality by design‐steered development and validation of analytical and bioanalytical methods for raloxifene: Application of Monte Carlo simulations and variance inflation factor

“…Standard drug solutions, each containing 25 μg mL −1 of RLX, were mixed with an equal volumetric proportion of 0.1 N HCl and 0.1 N NaOH, representing acidic and alkaline media, respectively, and were kept aside for a period of 4 h, until further analysis. After elapsing a time duration of 4 h, the samples were neutralized with 0.1 N NaOH and 0.1 N HCl, and estimation of RLX was performed using the HPLC procedure developed by our group (Sowjanya et al, 2012).…”

“…An equivalent volume of a standard fixed drug concentration (i.e. 25 μg mL −1 ) and hydrogen peroxide (H 2 O 2) solution (20%, v/v) was kept for 4 h, after which, the sample was subjected to HPLC analysis (Saini et al, 2012; Sowjanya et al, 2012).…”

“…An equivalent volume of a standard fixed drug concentration (i.e. 25 μg mL À1 ) and hydrogen peroxide (H 2 O 2) solution (20%, v/v) was kept for 4 h, after which, the sample was subjected to HPLC analysis (Saini et al, 2012;Sowjanya et al, 2012). The matrix effect was estimated for exploring the influence of proteins in blood plasma on varied RLX levels in the biological samples using Equation (1).…”

Spectrophotometric and Chromatographic Methods for the Estimation of Raloxifene Hydrochloride in Bulk and Pharmaceutical Formulations

“…7 [2] described HPLC method for the analysis of RXF in presence of its related substances using C8 as stationary phase and a movile phase of a solution of 9.0 g/L potassium dihydrogen phosphate adjusted to pH 3.0 with phosphoric acid and acetonitrile in the ratio of (70: 30 v/v). Several methods have been reported for the analysis of raloxifene hydrochloride in pharmaceutical dosage form including spectrophotometry [3][4][5][6][7], chromatography [8][9][10][11][12][13][14][15], electrochemistry [16] and capillary electrophoresis [17].…”

“…Mean ± SD of five blind concentrations(5,8,11,14,17 µg/mL) of RXF within the concentration range. Mean / RSD of triplicate determination of three concentrations (4, 9, 14 µg/mL) of RXF (n=9).…”