title: Stability-indicating RP-LC method for the determination of vildagliptin and mass spectrometry detection for a main degradation product.
abstract: A simple, precise and stability-indicating reversed-phase liquid chromatography method was developed and validated for the determination of vildagliptin (VLG) in pharmaceutical dosage form. The chromatographic separation was obtained within 6 min and was linear in the range of 20-80 µg/mL (r(2) = 0.9999). Limit of detection and limit of quantitation were 0.63 and 2.82 µg/mL, respectively. The method was validated in accordance with International Conference on Harmonization acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suitability. Stress studies were carried out and no interference of the degradation products was observed. The excipients did not interfere in the determination of VLG. Furthermore, the main degradation product obtained from the stress studies (thermal, oxidative and alkaline hydrolysis) was evaluated for mass spectrometry and its molecular structure was predicted. The proposed method was successfully applied for the quantitative analysis of VLG in tablet dosage form, which will help to improve quality control and contribute to stability studies of pharmaceutical tablets containing this drug.
authors.affiliation: Postgraduate Program in Pharmaceutical Sciences, Federal University of Rio Grande do Sul, Porto Alegre-RS, Brazil. amandatbarden@gmail.com
authors.forename: Amanda Thomas
authors.initials: AT
authors.lastname: Barden
authors.forename: Bárbara
authors.initials: B
authors.lastname: Salamon
authors.forename: Elfrides Eva Sherman
authors.initials: EE
authors.lastname: Schapoval
authors.forename: Martin
authors.initials: M
authors.lastname: Steppe
mesh_terms: D000218:Adamantane / Q000031:analogs & derivatives* / Q000032:analysis; D056148:Chromatography, Reverse-Phase / Q000191:economics / Q000379:methods*; D054873:Dipeptidyl-Peptidase IV Inhibitors / Q000032:analysis*; D004355:Drug Stability; D006868:Hydrolysis; D057230:Limit of Detection; D016014:Linear Models; D009570:Nitriles / Q000032:analysis*; D010084:Oxidation-Reduction; D004364:Pharmaceutical Preparations / Q000737:chemistry; D011759:Pyrrolidines / Q000032:analysis*; D013607:Tablets; D000077597:Vildagliptin
chemical_list: D054873:Dipeptidyl-Peptidase IV Inhibitors; D009570:Nitriles; D004364:Pharmaceutical Preparations; D011759:Pyrrolidines; D013607:Tablets; D000077597:Vildagliptin; D000218:Adamantane