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Simultaneous Determination of Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin in Bulk Drug and Formulation by UPLC Q-TOF-MS

Author(s):

Ramji Rathod, Faraat Ali, Amrish Chandra*, Robin Kumar, Meenakshi Dahiya and Gyanendra Nath Singh   Pages 1 - 12 ( 12 )

Abstract:


Background: A simple and sensitive Ultra Performance Liquid Chromatography-Mass Spectrometry method was developed and validated to measure the concentrations of Alogliptin (ALO), Linagliptin (LIN), Saxagliptin (SAX), and Sitagliptin (SIT) using Pioglitazone (PIO) as an internal standard.

Methods: Chromatographic separation of six gliptins was achieved on a C-18 column (100×2.1 mm, 2.7 µm) using a mobile phase consisting of Formic acid in the water, 0.1%v/v: Acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in positive ion mode. Targeted MS/MS mode on a QTOF MS was used to quantify the drug utilizing the transitions of 340.1(m/z), 473.2 (m/z), 316.2 (m/z), 408.1 (m/z), and 357.1 (m/z) for ALO, LIN, SAX, SIT and PIO respectively.

Results: As per ICH Q2R1 guidelines, a detailed validation of the method was carried out and the standard curves were found to be linear over the concentration ranges of 1516.0-4548.1 ng mL-1, 519.8-1559.4 ng mL-1, 1531.4-4594.3 ng mL-1and 1519.6-4558.8 ng mL-1 for ALO, LIN, SAX and SIT respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8 _ 0.76 % (GEM), 102.2 _ 1.59 % (LIN), 95.3 _ 2.74 % (SAX) and 99.2 _ 1.75 % (SIT) respectively.

Conclusions: The optimized validated UPLC QTOF-MS/MS method offered the advantage of shorter analytical times and higher sensitivity and selectivity. The optimized method is suitable for application in quantitative analysis of pharmaceutical dosage forms for QC laboratory.

Keywords:

UPLCQ-TOF-MS, Alogliptin, Linagliptin, Saxagliptin, and Sitagliptin

Affiliation:

Central Drugs Standard Control Organisation, Ministry of Health and Family Welfare, Govt. of India, New Delhi, Pharmaceutical Chemistry Division, Indian Pharmacopoeia Commission, Ministry of Health and Family Welfare, Govt. of India, Sector-23, Rajnagar, Ghaziabad, Uttar Pradesh-201002, Amity Institute of Pharmacy, Amity University, Noida, Uttar Pradesh, Pharmaceutical Chemistry Division, Indian Pharmacopoeia Commission, Ministry of Health and Family Welfare, Govt. of India, Sector-23, Rajnagar, Ghaziabad, Uttar Pradesh-201002, Pharmaceutical Chemistry Division, Indian Pharmacopoeia Commission, Ministry of Health and Family Welfare, Govt. of India, Sector-23, Rajnagar, Ghaziabad, Uttar Pradesh-201002, Pharmaceutical Chemistry Division, Indian Pharmacopoeia Commission, Ministry of Health and Family Welfare, Govt. of India, Sector-23, Rajnagar, Ghaziabad, Uttar Pradesh-201002



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