Liquid Chromatography/Electrospray Ionisation Tandem Mass Spectrometric Study of Sitagliptin and its Stressed Degradation Products

 

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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 identi­fied 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.

• References

• 1 Rao RN, Maurya PK, Khalid S. Development of a molecularly imprinted polymer for selective extraction followed by liquid chromatographic determination of Sitagliptin in rat plasma and urine. Talanta 2011; 85: 950-957
  CrossrefPubMedGoogle Scholar
• 2 Nirogi R, Kandikere V, Mudigonda K et al. Sensitive liquid chromatography tandem mass spectrometry method for the quantification of Sitagliptin, a DPP-4 inhibitor, in human plasma using liquid–liquid extraction. Biomedical Chromatography 2008; 22: 214-222
  CrossrefPubMedGoogle Scholar
• 3 El-Bagary RI, Elkady EF, Ayoub BM. Liquid chromatographic determination of Sitagliptin either alone or in ternary mixture with metformin and Sitagliptin degradation product. Talanta 2011; 85: 673-680
  CrossrefPubMedGoogle Scholar
• 4 Ravanello A, Schreiner Delgado L, Isa Pedroso Marcolino A et al. A Simple Stability-Indicating LC-UV Method to Assay Sitagliptin Phosphate in Tablets. Current Analytical Chemistry 2012; 8: 569-573
  CrossrefPubMedGoogle Scholar
• 5 Dubala A, Khatwal R, Kosaraju J et al. Bioanalytical method development and validation of Sitagliptin phosphate by RP-HPLC and its application to pharmacokinetic study. Int J Pharm Pharm Sci 2012; 4: 691-694
  PubMedGoogle Scholar
• 6 Sekaran CB, Rani AP. Development and validation of spectrophotometric method for the dtrmination of DPP-4 inhibitor, Sitagliptin, in its pharmactical preparations. Electica Quimica 2010; 35: 45-53
  PubMedGoogle Scholar
• 7 Sonune DP, Mahesh KM. Isolation, characterisation of degradation prodcts of sitagliptin and dvelopment of validated stability-indicating HPLC assay method for sitagliptin API and tablets. IJPSR 2013; 4: 3494-3501
  PubMedGoogle Scholar
• 8 Salim M, El-Enany N, Belal F et al. Micelle-enhanced spectrofluorimetric method for determination of sitagliptin and identification of potential alkaline degradation products using LC-MS. Luminescence 2013; DOI: 10.1002/bio.2503.
  PubMedGoogle Scholar
• 9 ICH . International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use. Validation of Analytical Procedures: Text and Methodology Q2 (R1) 2005;
  PubMedGoogle Scholar