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A validated new chiral LC method for the enantiomeric separation of vildagliptin

Ch.Surya Naga Malleswara Rao, G.Madhusudhan Reddy, K.Mukkanti, M.V.Suryanarayana, P.Pratap Reddy

A simple isocratic and chiral high performance liquid chromatographic method was developed for the determination of chiral purity of S-enantiomer of vildagliptin.Method involvedChiralpak-IC(250 x 4.6mm) column at constant room temperature using ethanol and diethylamine mixture in the ratio of 100: 0.1 (v/v) as mobile phase with a flowrate of 0.5 mLmin-1. The resolution (Rs) between the enantiomers was found to be greater than 4.0 and interestingly the R-enantiomer was eluted prior to the S-enantiomer in the developedmethod. The limit of detection (LOD) and limit of quantification (LOQ) of the R-enantiomerwas 0.15 and 0.5 µg mL-1, respectively, for 10 µL injection volume. The percentage recoveries of the R-enantiomer ranged from 95 to 105 in the bulk samples of vildagliptin. The test solution and mobile phase observed to be stable up to 48 h after the preparation. The method was validated as per International Conference on Harmonization (ICH) guidelines in terms of LOD, LOQ, linearity, precision, accuracy, specificity and robustness.