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.

Conclusion: 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.

背景：开发了一种简单而灵敏的超高效液相色谱-质谱法，并已使用吡格列酮（PIO）作为分析试剂来测量阿格列汀（ALO），利格列汀（LIN），沙格列汀（SAX）和西他列汀（SIT）的浓度。内部标准。

方法：在C-18色谱柱（100×2.1 mm，2.7μm）上，使用由甲酸，0.1％v / v：乙腈梯度洗脱的流动相进行色谱分离，分离出6种脂肪素。电喷雾电离（ESI）源以正离子模式运行。使用QTOF MS的靶向MS / MS模式通过340.1（m / z），473.2（m / z），316.2（m / z），408.1（m / z）和357.1（ m / z）分别用于ALO，LIN，SAX，SIT和PIO。

结果：如每ICH Q2R1准则，该方法的详细的验证进行并且发现标准曲线是线性的上方的1516.0-4548.1浓度范围纳克毫升^-1，519.8- 1559.4纳克毫升^-1，1531.4-4594.3分别用于ALO，LIN，SAX和SIT的ng mL ^-1和1519.6-4558.8 ng mL ^-1。精度和准确性结果均在可接受的范围内。平均回收率分别为98.8±0.76％（GEM），102.2±1.59％（LIN），95.3±2.74％（SAX）和99.2±1.75％（SIT）。

结论：经过优化，经过验证的UPLC QTOF-MS / MS方法具有分析时间更短，灵敏度和选择性更高的优点。优化后的方法适用于质控实验室药物剂型的定量分析。