Identification and Separation of the Degradation Products of Vildagliptin Tablets and Raw Material using LC-MS and NMR, and then Exploration  of the Corresponding Degradation Pathways

Enas Alqudah; Malak Abbadi; Sawsan Alqadoomi; Ibtihal Abo Hameda; Sharif Arar; Kamal Sweidan

doi:10.35516/jjps.v16i2.1535

Authors

Enas Alqudah Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.
Malak Abbadi Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.
Sawsan Alqadoomi Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.
Ibtihal Abo Hameda Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.
Sharif Arar Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.
Kamal Sweidan Department of Chemistry, School of Science, The University of Jordan, Amman, Jordan.

DOI:

https://doi.org/10.35516/jjps.v16i2.1535

Keywords:

Vilaglibtin, tablet form, excipients, forced, degradation, impurity profile, 2D-NMR

Abstract

A gradient high performance liquid chromatography (HPLC) method has been developed for the qualitative and quantitative analyses of vildagliptin related substances. This method is based on using of RP-C18 (250 × 4.6 mm×5µm) and gradient elution with phosphate buffer and methanol as mobile phase. Various forced degradation studies were conducted to establish an impurity profile for vildagliptin in the tablet formula. Three degradation products were produced upon exposing vildagliptin to different degradation conditions (acidic, basic, oxidative, photolytic, aqueous and thermal); their structures were characterized using LC-MS and NMR (¹H NMR, ¹³C NMR and DEPT) techniques. Some excipient components, examined in this study, had major effect towards producing any extra new degradation products.