title: Liquid chromatography/electrospray ionisation tandem mass spectrometric study of sitagliptin and its stressed degradation products.
abstract: A sensitive UPLC positive ion electrospray tandem mass spectrometry method was developed and validated for identification of degradation products of sitagliptin formed during stress study. Six of the major degradants were identi-fied with the proposed method. The separation of sitagliptin and its degradation products was achieved on a Acquity BEH C-18 column (50×2.1 mm, 1.7 µm) using a gradient programme. The mobile phase consists of solvent A (10 mM ammonium formate, pH 6.4 adjusted with formic acid) and solvent B (acetonitrile) and quantitative evaluation was performed at 267 nm with a flow rate of 0.15 mL min(-1). Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with International Conference on Harmonization (ICH) guidelines and can be used for routine analysis of sitagliptin formulations in quality control.
authors.affiliation: Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research, Hyderabad (NIPER- Hyderabad), Balanagar, Hyderabad, India.
authors.forename: C
authors.initials: C
authors.lastname: Vishnuvardhan
authors.affiliation: United States Pharmacopeia - India Private Limited, Research and Development Laboratory, ICICI Knowledge Park, -Turkapally, Shameerpet, Hyderabad, India.
authors.forename: P
authors.initials: P
authors.lastname: Radhakrishnanand
authors.affiliation: United States Pharmacopeia - India Private Limited, Research and Development Laboratory, ICICI Knowledge Park, -Turkapally, Shameerpet, Hyderabad, India.
authors.forename: S G
authors.initials: SG
authors.lastname: Navalgund
authors.affiliation: Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research, Hyderabad (NIPER- Hyderabad), Balanagar, Hyderabad, India.
authors.forename: N
authors.initials: N
authors.lastname: Satheeshkumar
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods; D004355:Drug Stability; D011719:Pyrazines / Q000737:chemistry*; D011786:Quality Control; D015203:Reproducibility of Results; D000068900:Sitagliptin Phosphate; D012997:Solvents / Q000737:chemistry; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods; D053719:Tandem Mass Spectrometry / Q000379:methods; D014230:Triazoles / Q000737:chemistry*
chemical_list: D011719:Pyrazines; D012997:Solvents; D014230:Triazoles; D000068900:Sitagliptin Phosphate