The number of drugs introduced into the market is increasing every year. These drugs may be either new entities or partial structural modification of the existing one. Often a time lag exists from the date of introduction of a drug into the market to the date of its inclusion in pharmacopoeias. Hence, standards and analytical procedures for these drugs may not be available in the pharmacopoeias. It becomes necessary, therefore to develop newer analytical methods for such drugs.  Hence the present research work was designed to develop a new RP HPLC method for the simultaneous estimation of Ezetimibe and Glimepiride in pharmaceutical dosage form. The wavelength of maximum absorption (λ_max) of the drug, 10 μg/ml solution of the drugs in methanol were scanned using UV-Visible spectrophotometer within the wavelength region of 200–400 nm against methanol as blank. The Isosbestic point was found to be 228 nm for Ezetimibe and Glimipride combination. Efficiency was more and resolution was good with mobile phase Triethylamine: Methanol (30:70) at 228 nm. Asymmetry was good. Hence the method was optimized. The amount of Ezetimib and Glimipride present in the taken dosage form was found to be 99.94% and 99.89% respectvely.

Key words: Ezetimibe, Glimepiride, RP HPLC, simultaneous estimation, Isosbestic point.