Abstract

*Dara.Varun Kumar and Kumaraswamy.Gandla

ABSTRACT

A simple, fast, accurate and precise UV-spectroscopic method and RP-HPLC method were developed and validated for the estimation of Nilotinib/Gemcitabine per ICH guidelines. Acetonitrile and water (50:50) was used as the solvent. The ? max of Nilotinib/Gemcitabine was found to be 242 nm and it was proved linear in the concentration range of Nilotinib 0.5-3?g/ml and for Gemcitabine 1-6?g/ml with a correlation coefficient value of 0.999. Accuracy studies of UV-spectroscopy method was performed at three different levels, i.e., 50%, 100%, and 150% and recovery was found to be in the range of 99.6 to 100.8% for Nilotinib and the range of 98.3 to 101.2% for Gemcitabine respectively. The Limit of Detection (LOD) and Limit of Quantification (LOQ) were found to be 0.217 and 0.658 ?g/ml for Nilotinib and 0.103 and 0.312 f or Gemcitabine RP-HPLC method was developed by using Acetonitrile: water, 0.1% ortho phosphoric acid (50:50). The method was developed in Eclipse C18 column (100 mm × 4.6 mm, 3.5?m particle size). In RP-HPLC method was found to be linear in the range of Nilotinib/Gemcitabine is 0.25-1.5?g/ml with a correlation coefficient value of 0.999. The accuracy studies of RP-HPL C method was performed at three different levels, i.e., 50%, 100%, and 150% and recovery was found to be in the range of 98.24 t o 100.3% for Nilotinib and the range of 98.18 to 99.98% and for Gemcitabine respectively. The limit of detection (LOD) and Li mit of Quantification (LOQ) were found to be 0.0421 and 0.1276 ?g/ml for Nilotinib and 0.047.and 0.1424 ?g/ml for Capecit abine for RP-HPLC method. The % RSD is <2% which indicates the accuracy and precision of the method. The abo ve method was a rapid tool for routine analysis of Nilotinib/Gemcitabine in the bulk and in the pharmaceutical dosage form.