Abstract
Objective of the proposal was to establish rapid, economical, and robust liquid chromatographic procedure to perform quality control of a pharmaceutical preparation containing amlodipine and celecoxib using an experimental design. The proposed new high-performance liquid chromatography (HPLC) procedure involves isocratic separation using sodium phosphate buffer (pH 5.6): acetonitrile: methanol in a ratio 30:55:15 (v/v) as the mobile phase on a Zorbax C18 (150 mm) reverse-phase (RP)-HPLC column. The analysis was performed at 25 degrees C, using a flow rate of 1.2 mL/minute. The column elutes were detected at 239 Tun and etoricoxib has been selected as an internal standard (IS). The calibration curve exhibited good linearity in the range of 5-30 mu g/mL of amlodipine and 50-500 mu g/mL of celecoxib with a good correlation coefficient (r(2) > 0.999). The precision and accuracy were presented in terms of%RSD and%RE and were in an acceptable range ( <2). The accuracy of the suggested procedure was established by the results of recovery studies, executed using a standard addition method. A robustness test was performed using fractional factorial design with three major contributing factors. The pH of the mobile phase and flow rate demonstrated a substantial effect on the peak area ratio of amlodipine, whereas the percent of acetonitrile and the flow rate together exhibited an effect on the peak area ratio of celecoxib. This validated, robust analytical method has been utilized to quantify amlodipine and celecoxib from formulations with large concentration differences. Further, the comparison of results with reported methods indicated that no significant difference was observed in terms and accuracy and precision.