Original Articles
D Pavan Kumar, T Naga Jhansi,
Abstract
Reversed phase chiral HPLC method for separation enantiomers of sitagliptin was developed and validated. These sitagliptin isomer were resolved on a chiralpak IC (250 mm x 4.6 mm, 5 µm) column by using liquid mobile phase of 10 mM ammonium acetate with 0.05% Di ethyl amine –acetonitrile (40:60 v/v).Both enantiomers are well resolved with the resolution of less than 3.0. Newly developed method was verified by validating according to ICH guidelines. Method was linear over the concentration range 0.0003 mg mL-1 to 0.0045 mg mL-1(r2 =0.9991). The detection level and quantification level of the (s)-enantiomer were identified to be 0.0001mg mL-1 and 0.0003 mg mL-1,respectively for 20 µL injection volume. (S)-enantiomer recovery is in the ranged of 95.7 to 101.7 in API samples of sitagliptin. Both sample solution and mobile phase were stable for 48 hrs in this method. The final optimized method conditions were well established the separation of (s)-enantiomer from sitagliptin and demonstrated that the method is reproducible, accurate and robust for the quantitate estimation of enantiomeric purity of sitagliptin in API samples.