Abstract

ANALYTICAL METHOD DEVELOPMENT AND VALIDATION PROTOCOL FOR ALISKIRENHEMIFUMARATE AND IRBESARTAN

Prashant Kumar Katiyar* and Dr. R. S. Ghosh

Abstract

Reversed-phase high-performance liquid chromatography method was developed and validated for the simultaneous estimation of Aliskirenhemifumarate and Irbesartan. Chromatographic separation was achieved with a Shimadzu’s high performance liquid chromatography C18 column (150X4.6 mm, 5mm) Buffer (Potassium Dihydrogen Orthophosphate pH:3.5):methanol: Acetonitrile with a mobile phase of ratio 45:20:50v/v. The flow rate was set at 1ml/min and the detection wavelength was 271 nm and 236 nm respectively. Quality by design approach was employed for optimization of method parameters like proportion of mobile phase, concentration of buffer and a model highlighting the design space was generated. This developed chromatographic method gave well resolved symmetric peaks. Aliskiren and Irbesartan were eluted at 2.29 and 3.35 min, respectively. This method was validated according to International Conference on Harmonisation Q2(R1) guideline. The method was linear in range of 01 to 05 𝜇g/mL for Aliskirenhemifumarate and 01 to 05 𝜇g/mL of Irbesartan by RP-HPLC and the linearity study showed the regression co-efficient as 0.9994 and 0.996 for aliskiren hemifumerate and irbesartan respectively and The linearity graph of both drugs was obtained in a range of 5 to 25 μg/ ml for Aliskiren hemifumerate and 2 to 10μg/ mL for Irbesartan by UV Spectroscopy. The sample recoveries were in good agreement with the respective label claim, which suggested non-interference from formulation additives in the estimation.

Keywords: Analytical Method Development, RP-HPLC, Simultaneous Equation Method, Aliskiren and Irbesartan.