A RAPID SENSITIVE AND ACCURATE LCMS METHOD FOR THE DETERMINATION OF MUTAGENIC IMPURITIES IN MOXIFLOXACIN HCL

Abstract

A quantitative method was developed and then validated for two genotoxic impurities (GTS-STG-1A and GTS/STG-1B) in moxifloxacin hydrochloride API samples using the LC–MS approach. The analytes (GTS-STG-1A and GTS/STG-1B) were separated on XDB-column [C8; Eclipse; 5 µm particle dimension; 150 mm length; and ID of 4.6 mm] using a blend of solvent systems ‘A’ (10 mM strength ammonium formate) and ‘B’ (pure acetonitrile) in a gradient pattern elution. The GTS-STG-1A and GTS/STG-1B were detected by positive mode electrospray ionization. The transitions at m/z 332.1–286.2 and 344.2–298.4 were used for GTS-STG-1A and GTS/STG-1B quantitative analysis. Better linearity for the concentration ranges of 0.3863 ppm to 5.7938 ppm for GTS-STG-1A and 0.3786 ppm to 5.6790 ppm for GTS/STG-1B was obtained. The accuracies (94.6% to 99.35 for GTS-STG-1A and 83.25% to 105.9% for GTS-STG-1B) and precisions (1.40% for GTS-STG-1A and 4.30% for GTS-STG-1B) fell within the allowable threshold. The GTS-IA and GTS-IB demonstrated adequate stability under-examined conditions. By keeping track of the GTS-STG-1A and GTS/STG-1B content in the moxifloxacin hydrochloride API during the experiment, the usefulness of the LC-MS technique was shown.