Abstract : A simple, rapid, precise and reliable RP-HPLC method was developed for estimation of Voglibose (VOG) and Mitiglinide calcium hydrate (MGN) in pharmaceutical dosage form. The method is based of precolumn derivatization of Voglibose with 9-Fluorenylmethyloxycarbonyl chloride (FMOC - chloride) due to lack of chromophoric group it cannot directly estimated by UV detector in RP-HPLC method. Precolumn derivatization (PCD) conditions were optimized by evaluating the parameters such as concentration of borate buffer, concentration of FMOC-Cl and reaction time of derivatization. The chromatographic separation was achieved on Cosmosil BDS C18 (15 cm × 0.46 cm id, 5µm particle size) column using phosphate buffer (pH 4.0) and methanol (30:70) as mobile phase. Detection was carried out at 233 nm using UV detector. The retention time of Voglibose and Mitiglinide calcium hydrate were found to be 5.233 min and 3.580 min respectively. The developed method was validated for parameters such as accuracy, precision, linearity and solution stability.