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Liquid chromatography tandem mass spectrometry (LC-MS/MS) method for the determination of Vildagliptin in rat plasma

Sakthimanigandan K., Ganesh M., Kanthikiran V., Sivakumar T., Jang H.

Acta Chromatographica

2015

Vol. 27, no. 2

295--307

A new sensitive and validated liquid chromatography electro spray ion-tandem mass spectrometry (HPLC-ESI-MS/MS) method for the quantification of Vildagliptin (VG) in rat plasma has been developed and validated using repaglinide (RG) as an internal standard (IS). The analytes were extracted by liquid-liquid extraction using ethyl acetate. Elution of the VG and IS was achieved on a reverse phase Betasil (C18 50 mm 4.6 mm ID, 5 μ) column with an isocratic mobile phase composed of acetonitrile: 2 mM ammonium acetate (90:10 v/v). The analytes monitored in the Multiple Reaction Monitoring (MRM) mode were m/z 304.2→154.0 and 453.3→230.3 for VG and RG, respectively. The calibration curve was linear in the range of 1.57–501.21 ng/mL for VG with lower limit of quantification 1.57 ng/mL. The intra run and inter run precision values are within 11.70% for VG at LOQ level.

Validated HPLC method for analysis of oxaprozin in a formulation

Ganesh M., Thangabalan B., Patil R., Thakur D., Saravana Kumar A., Vinoba M., Ganguly S., Sivakumar T.

Acta Chromatographica

2008

Vol. 20, no. 2

165-173

A rapid, simple and validated reversed-phase high-performance liquid chromatographic method has been developed for analysis of oxaprozin in pharmaceutical dosage forms. Oxaprozin was separated on an ODS analytical column with a 45:55 (v/v) mixture of acetonitrile and triethanolamine solution (5 mM, pH 3.5 š 0.05, adjusted by addition of 85% phosphoric acid) as mobile phase at a flow rate of 2.0 mL min-1. The effluent was monitored by UV detection at 254 nm. Calibration plots were linear in the range 160 to 240 µg mL-1 and the LOD and LOQ were 14.26 and 41.21 µg mL-1, respectively. The high recovery and low relative standard deviation confirm the suitability of the method for routine QC determination of oxaprozin in tablets.