A Robust QBD Based High-Performance Thin-Layer Chromatographic Method for the Estimation of Aspirin, Clopidogrel Bisulphate and Rosuvastatin Calcium in a Pharmaceutical Formulation Using Experimental Design

Background: The article describes how a new robust HPTLC method was developed to separate and quantify aspirin, clopidogrel bisulphate and rosuvastatin calcium in a fixed dose combination present in a capsule dosage form using quality by the design approach.

Methods: A central composite experimental design has been framed and results were analysed by using a modern statistical technique called response surface methodology in order to study the effects of chromatographic chamber saturation time, volumes of ionic modifier and mobile phase ratio on Rf value and band shape.
Results: The Rf value predicted for aspirin, clopidogrel bisulphate and rosuvastatin calcium was in between 0.3 and 0.84. After optimization, the chromatographic conditions were 20 min saturation time and 7:3:0.2 v/v/v as the ratio of ethyl acetate, chloroform and pH modifier (Glacial Acetic acid) as a mobile phase. The LOD was found 45.2 ng band-1 15.9 ng band-1 and 6.8 ng band-1; and the LOQ was found 150.7 ng band-1 53.05 ng band-1 and 22.7 ng band-1 for AS, CL and RO respectively Conclusion: The optimized HPTLC method was validated according to (ICH) guideline Q2 (R1). The results prove that QbD concept effectively optimizes HPTLC methods with the minimum number of experiments. Developed HPTLC method was successfully applied for commercial samples of aspirin, clopidogrel bisulphate and rosuvastatin calcium in triple combination capsule dosage form.