VALIDATED UPLC/Q-TOF-MS METHOD FOR SIMULTANEOUS DETERMINATION OF ACECLOFENAC, PARACETAMOL, AND THEIR DEGRADATION PRODUCTS IN TABLETS

摘要

A fast, sensitive, and specific ultra-performance liquid chromatography/ quadrupole time-of-flight mass spectroscopy (UPLC/ Q-TOF-MS) method has been developed and validated for the simultaneous determination of aceclofenac, paracetamol, and their major degradation products in tablets. Diclofenac and para-aminophenol as the potential degradation product of aceclofenac and paracetamol, respectively, were analyzed. The chromatographic separation was achieved on Acquity UPLC BEH C_(18) (100.0x 2.1 mm, 1.7 um) column using isocratic mobile phase consisting of acetonitrile-2 mM ammonium acetate (40:60, v/v) at a flow rate of 0.25 mL/min. The Q-TOF mass spectrometer was operated in positive ionization mode and quantitation was done using the MS/MS transitions m/z 354.07 -> 215.07for aceclofenac, 296.23-> 214.06 for diclofenac, 152.07-> 110.06 for paracetamol, and 110.07-> 65.04 for para-aminophenol. The elution of aceclofenac, diclofenac, paracetamol, and para-aminophenol occurred at 1.50, 1.05, 0.61, and 1.61 min, respectively. The calibration curves were linear over the concentration range of 1-1000 ng/mL for aceclofenac and paracetamol, 0.01-1 ng/mL for diclofenac and 0.01-5 ng/ mL for para-aminophenol. The developed method was validated according to ICH guidelines. The proposed method can be applied for determination of aceclofenac and paracetamol during routine quality control analysis and in stability studies to monitor the level of their degradation products in bulk drugs or in pharmaceutical formulations.