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Development and Validation of a Rapid and Sensitive Method for the Simultaneous Estimation of Gemigliptin and Teneligliptin in Bulk and Dosage Forms by Using Liquid Chromatography-Tandem Mass Spectrometry

Author(s):

Ramji Rathod, Amrish Chandra*, Faraat Ali*, Anuj Prakash, Robin Kumar and Gyanendra Nath Singh   Pages 1 - 8 ( 8 )

Abstract:


Background: A simple and sensitive ultra-performance liquid chromatography-mass spectrometry method was developed and validated to measure the concentrations of gemigliptin (GEM) and teneligliptin (TEN) using pioglitazone (PIO) as an internal standard.

Methods: Chromatographic separation of two gliptins was achieved on a C-18 (100 mm X 2.1 mm, 2.7 µm) column using a mobile phase consisting of formic acid in water (0.1 % v/ v): acetonitrile in gradient elution. Electrospray ionization (ESI) source was operated in positive mode (ionization). Targeted MS-MS mode on a quadrupole time of flight (Q-TOF) mass spectrometer was used to quantify the drugs utilizing the mass transitions of 490.1 (m/z), 427.2 (m/z) and 357.1 (m/z) for GEM, TEN 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 between over the concentration ranges of 509.8-1529.4 ng mL-1 and 510.6-1531.7 ng mL-1 for GEM and TEN respectively. Precision and accuracy results were within the acceptable limits. The mean recovery was found to be 98.8± 0.76 % (GEM) and 98.6 ±0.98 % (TEN) respectively.

Conclusions: The optimized validated UPLC-QTOF (MS-MS) method offered the advantage of shorter analytical times and higher sensitivity and selectivity to the nanogram level.

Keywords:

UPLC-QTOF-MS, Liquid chromatography, Gemigliptin, Teneligliptin, DPP-4 inhibitor

Affiliation:

Central Drugs Standard Control Organisation, Ministry of Health and Family Welfare, Govt. of India, New Delhi, 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, 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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