STRUCTURAL IDENTIFICATION AND QUANTITATIVE DETERMINATION OF ANTI-DIABETIC DRUGS BY UPLC/Q-TOF-MS TECHNIQUE
Hamid Khan*
ABSTRACT
In the presented work the ultra-performance liquid chromatographic/quadrupole time-of-flight mass spectrometric (UPLC/Q-TOF-MS) method has been developed for structural identification and quantification of three anti-diabetic drugs namely metformin, glimepiride and pioglitazone. For identification of drugs, the Q-TOF mass spectrometer was operated in positive ionization mode and quantification was done using the MS/MS transitions at m/z 130.0 to 71.0 for metformin, 491.00 to 352.00 for glimepiride, and 357.00 to 134.00 for pioglitazone. The chromatographic separation was achieved on Acquity UPLCTM BEH C18 (100.0 × 2.1 mm, 1.7μm) column using isocratic mobile phase consisting of acetonitrile-2mM ammonium acetate (50:50, v/v) at a flow rate of 0.25 mL/min. The elution of metformin, glimepiride and pioglitazone 0.50, 1.40, and 2.22 min, respectively. The calibration curves were linear over the concentration range of 1-1000 ng/mL for all the drugs. The developed method was validated according to ICH guidelines. The fragmentation mechanisms of drugs were established by the study of their mass spectra.
Keywords: UPLC/Q-TOF-MS, Metformin, Glimepiride, Pioglitazone.
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