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 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
found to be within the acceptable limits. The mean recovery was found to be 98.8± 0.76 % (GEM)
and 98.6 ±0.98 % (TEN), respectively.
Conclusion: The optimized validated UPLC-QTOF (MS-MS) method offered the advantage of
shorter analytical times and higher sensitivity and selectivity to the nanogram level.