Stability-indicating liquid chromatographic method for determination of saxagliptin and structure elucidation of the major degradation products using LC-MS.

Abstract

A new, simple, selective, reproducible and sensitive stability-indicating liquid chromatographic method was developed and subsequently validated for the determination of saxagliptin (SXG). SXG was subjected to oxidation, thermal, acid hydrolysis, alkali hydrolysis and photodegradation according to ICH guidelines. The major degradation products were separated from the pure drug and the proposed structures' elucidation was performed, using an LC-MS technique. Isocratic chromatographic elution was achieved on a Symmetry(®) C18 column (150 × 4.6 mm, 5 µm), using a mobile phase of potassium dihydrogen phosphate buffer (pH 4.6)-acetonitrile-methanol (40 : 30 : 30, v/v/v) at a flow rate of 1 mL min(-1) with UV detection at 208 nm. Linearity, accuracy and precision were found to be acceptable over the concentration range of 25-400 µg mL(-1). All the results were statistically compared with the reference method, using one-way analysis of variance. The developed method was validated and proved to be specific and accurate for quality control of SXG in pharmaceutical dosage form.