Method Development and Validation Cilnidipine and Chlorthalidone in Bulk and In Its Pharmaceutical Dosage Forms by Using HPLC as Per ICH Guidelines

P.S Bhargav¹, Gampa Vijay Kumar^2
1KGR Institute of Technology and Management, Rampally, Kesara, Rangareddy, Telangana, India.
²Professor and Head, Dept. of Pharmacy, KGR Institute of Technology and Management, Rampally, Kesara, Rangareddy, Telangana, India.

ABSTRACT
New method was established for simultaneous estimation of Clinidipine and Chlorthalidone  by RP-HPLC method. The chromatographic conditions were  successfully developed for the separation of Clinidipine and Chlorthalidone  by using Zodiac sil RPC18 4.6×250mm 5µm, flow rate was 1.2 ml/min, mobile phase ratio was (70:30 v/v) methanol:Phosphate bufferpH 3 (pH was adjusted with orthophosphoricacid), detection wavelength was 240nm. The retention times were found to be 2.746 mins and 3.608 mins. The % purity of Clinidipine and Chlorthalidone  was found to be 101.27% and 99.97% respectively. The system suitability parameters for Clinidipine and Chlorthalidone  such as theoretical plates and tailing factor were found to be 4668, 1.3 and 6089 and 1.2, the resolution was found to be 6.0. The analytical method was validated according to ICH guidelines (ICH, Q2 (R1)). The linearity study n Clinidipine and Chlorthalidone was found in concentration range of 50µg-250µg and 5µg-50µg and correlation coefficient (r²) was found to be 0.999 and 0.999, % recovery was found to be 99.56% and 99.48%, %RSD for repeatability was 0.2 and 0.2, % RSD for intermediate precision was 0.2 and 0.1respectively. The precision study was precise, robust, and repeatable.LOD value was 3.17 and 5.68, and LOQ value was 0.0172 and 0.2125 respectively. Hence the suggested RP-HPLC method can be used for routine analysis of Clinidipine and Chlorthalidone in API and Pharmaceutical dosage form.
Keywords: Zodiac sil RPC18 column, Clinidipine and Chlorthalidone, RP-HPLC