Title:Stability Indicating Method for Known and Unknown Impurities Profiling for Vildagliptin in Vildagliptin Tablet
Volume: 17
Issue: 10
Author(s): Nitin Mahajan*, Suparna Deshmukh and Mazhar Farooqui
Affiliation:
- Post Graduate and Research Centre, Department of Chemistry, Maulana Azad College of Arts, Science and Commerce, Aurangabad, Maharashtra,India
Keywords:
Impurity profiling, degradation products, analytical method development, analytical method validation, HPLC, related
substances, vildagliptin.
Abstract:
Background: Vildagliptin is a drug for the treatment of diabetes. DPP-IV inhibitor represents
a new class of oral antihyperglycemic agents to treat patients with type 2 diabetes. Several
RP-HPLC methods have been reported to determine Vildagliptin alone. However, it has been noted
that there are no available stability-indicating methods in pharmacopeias (USP/BP/EP/JP) nor in
the available literature to quantify known and unknown impurity patterns for vildagliptin in
vildagliptin tablets.
Objective: The aim of this study is to develop a new single, sensitive, robust and specific gradient
RP-HPLC method to quantify known and unknown impurities and degradants of Vildagliptin in
Vildagliptin tablets.
Methods: Chromatographic separation has been accomplished on the Hypersil ODS column (250 x
4.6) mm, 5 μm with a mobile phase consisting of a mixture of Perchloric acid Buffer, methanol,
acetonitrile and Triethylamine delivered at a flow rate of 1.0 mL minute-1 and the detection wavelength
210 nm. The developed method was validated as per ICH guidelines.
Results: Vildagliptin was found degraded significantly under oxidative and alkaline stress conditions.
The degradation products were well resolved from Vildagliptin and its impurities. An analytical
method was found linear, accurate and precise from LOQ (Limit of Quantification) level to
150% of impurity specification limit (0.5%).
Conclusion: The method found sensitive, rapid and accurate quantification of known, unknown impurities
and degradants. The peak purity results confirmed that the Vildagliptin peak was homogeneous
and pure in all stress samples, thus proving the stability-indicating nature of the method.