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 water, 0.1%v/v: acetonitrile in gradient elution.
Electrospray ionization (ESI) source was operated in the 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.
The Development and Validation of a Novel Designer Benzodiazepines Panel by LC–MS-MS