Design of experiment driven ecofriendly RP-HPLC for simultaneous determination of Cilnidipine and Metoprolol succinate

Abstract

The analytical community prioritizes adopting green techniques due to concerns over the environmental impact of chemical research. This study employs an integrated experimental strategy, combining the concept of design of experiment (DOE) and green analytical chemistry (GAC), to establish a robust, green RP-HPLC approach for the simultaneous estimation Cilnidipine (CIL) and Metoprolol succinate (MET). For method optimization, a central composite design (CCD) was implemented. Separation utilized Inertsil ODS 3 column (250 mm x 4.6 mm, 5 μm), with gradient mobile phase (ethanol: 17.65% at 0 min, 75.5% at 3 min) and phosphate buffer, flowing at 1 ml/ min. Detection wavelength at 230 nm. Column temperature (35±1°C), and injection volume 5 μL. Retention times: MET (4.672 min), CIL (7.457 min). The linearity was established over the range of 7-13 μg/ml for CIL and 35-65 μg/ml for MET. The values obtained for LOD and LOQ are 0.819 and 2.482 μg/ml (CIL) respectively, 3.875 and 11.743 μg/ml (MET). As per ICH Q14, the technique has been validated. Finally the green nature was examined by GAPI, AES and AGREE. Method found to be ecofriendly, simple and robust for simultaneous CIL and MET estimation in pharmaceutical formulations, easily adaptable for routine analysis.

GRAPHICAL ABSTRACT

Keywords:

• Cilnidipine
• Central composite design
• Greenness profile
• Metoprolol succinate
• Stability indicating