Abstract

METHOD DEVELOPMENT AND VALIDATION OF ALISKIREN HEMIFUMARATE IN BULK DRUG MANUFACTURING OF ACTIVE PHARMACEUTICALS INGREDIENT BY REVERSE PHASE HIGH PRESSURE LIQUID CHROMATOGRAPHY

N.H. Eswara Prasad, Dr. K. Basavaiah*, Dr. B.M.Rao, N.V.N.B. Srinivasa Rao, Y.V. Sunil Kumar and Dharmasoth Rama Devi

ABSTRACT

The main study depicts the development of a validated reverse phase high performance liquid chromatographic (RPHPLC) method for the determination of aliskiren hemifumarate related substances in active pharmaceutical ingredient. The method was developed by using the gradient system. Acetonitrile, HPLC grade water, methanol and buffer were used as chemicals and reagents. The buffer was prepared using the mixture of 0.02 M solid ortho phosphoric acid and 0.02M tetra-n-butyl ammonium hydrogen. Mobile phase A was prepared using buffer: methanol: acetonitrile in the ratio of 80:10:10% (v/v) and mobile phase B was prepared using buffer and acetonitrile in the ratio of 25:75% (v/v). Diluent was prepared by mixing the volumes of solid orthophosphoric acid and acetonitrile in the ratio of 80:20. Successful elution of aliskiren hemifumarate was achieved in water symmetry C18 column with 150 x 4.6 mm internal diameter and 3μm particle size.The flow rate was set to 0.8 ml/min with the responses measured at 228 nm using Agilent 1200series liquid chromatograph equipped with variable wave length UV-detector. The retention time of aliskiren hemifumarate was found to be 16.244 minutes. Linearity was established for aliskiren hemifumarate in the range of 25-150 % with correlation coefficient 0.9994. Considering all the results, it is concluded that the developed and validated method can be suitable for the regular quality control determination of aliskiren hemifumarate in bulk as well as pharmaceutical dosage form. The developed RPHPLC method was validated with respect to system suitability, system precision, specificity (interference of diluent), linearity, limit of detection & limit of quantitation, method precision, range, accuracy & test solution stability.

Keywords: Aliskiren hemifumarate, Reverse phase high performance liquid chromatographic (RPHPLC), Validation, Pharmaceutical dosage form.