Systematical approach in evaluation of LC method for determination of raloxifene hydrochloride and its impurities employing experimental design

Abstract

Method validation presents a detailed investigation of analytical method and provision of the evidence that the method, when correctly applied, produces results that fit to the purpose. In order to achieve the method validation scope efficiently, experimental design presents a very useful tool. The greatest benefits of such approach could be seen in robustness testing through the provision of very useful data about the control of the chromatographic system during the routine application. In this paper, robustness testing of the LC method proposed for the determination of raloxifene hydrochloride and its four impurities was done employing Plackett–Burman design. Applying this design, the effect of five real factors (acetonitrile content, sodium dodecyl sulfate content, column temperature, pH of the mobile phase and flow rate) on the corresponding resolution factors was investigated through twelve experiments. Furthermore, the insignificance intervals for significant factors were calculated and the parameters for system suitability tests were defined. Eventually, the other validation parameters were tested and the effectiveness of the proposed analytical method with a high degree of accuracy was confirmed.

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

“…Several chromatographic methods were reported for the analysis of RXF, but all those methods suffered from critical conditions, either by applying gradient elution [9,12,13]; or by using a mobile phase containing controlled pH buffer [8,10,15] which may affect the life time of the column. So the aim of this work was to develop and validate accurate and precise HPLC method using isocratic elution and a simple mobile phase.…”

“…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].…”

Development and validation of stability indicating RP-HPLC method for the determination of related substances in Raloxifene hydrochloride tablets dosage forms

“…Literature view report that different spectrophotometric methods are available for raloxifene determination (Sivasubramanian and Pavithra, 2006;Kalyanaramu and Raghubabu, 2011;k Basavaiah et al, 2008) and through Reversed-Phase HPLC in dosage and bulk drug form (Salazar et al, 2015;Suneetha and Rao, 2010;Kumar et al, 2011). Plackett-Burman design is used for the evaluation of raloxifene hydrochloride and its impurities by a new LC Validation method (Stojanović et al, 2013). UPLC method to analysis raloxifene and its corresponding impurities in drug and dosage form reported Saini et al (2012).…”