CHEMOMETRIC-ASSISTED SPECTROPHOTOMETRIC AND HPLC METHODS FOR THE SIMULTANEOUS ANALYSIS OF ATORVASTATIN CALCIUM AND EZETIMIBE

Abstract

This study aimed to develop new analytical strategies for the simultaneous determination of atorvastatin calcium (ATVC) and ezetimibe (EZE) in pharmaceutical formulations. The proposed methods included a chemometric approach using the partial least squares (PLS) technique with spectrophotometric data, first derivative zero-crossing, ratio spectra first derivative, and HPLC-DAD. PLS analysis was conducted using specialized software, with calibration performed in the 223–280 nm range at Δλ = 4 nm intervals. In the first derivative zero-crossing method, absorbance values at 245.2 nm for ATVC and 224.8 nm for EZE were used. The ratio spectra first derivative method quantified ATVC at 232.6 nm and EZE at 223.1 nm. HPLC-DAD analysis was carried out using an XBridge C18 column with a mobile phase of 20 mM NaH₂PO₄:ACN (50:50 v/v), (240 nm, 1.0 mL/min). The linearity ranges were 1–20 μg/mL, 2–10 μg/mL, and 0.05–1.0 μg/mL, respectively. The methods were validated according to ICH guidelines, with no significant statistical differences observed (ANOVA, p > 0.05). Recovery from tablet formulations ranged from 95.43% to 102.28%. The PLS technique was highlighted as an environmentally friendly analytical approach. These validated methods demonstrated high sensitivity, accuracy, and reproducibility for routine pharmaceutical analysis.