title: An integrated method for degradation products detection and characterization using hybrid ion trap/time-of-flight mass spectrometry and data processing techniques: Application to study of the degradation products of danofloxacin under stressed conditions.
abstract: A new strategy using hybrid ion trap/time-of-flight mass spectrometry coupled with high-performance liquid chromatography and post-acquisition data mining techniques was developed and applied to the detection and characterization of degradation products of danofloxacin. The degradation products formed under different forced conditions were separated using an ODS-C18 column with gradient elution. Accurate full-scan MS data were acquired in the first run and processed with the combination of extracted ion chromatograms and LC-UV chromatograms. These processes were able to find accurate molecular masses of possible degradation products. Then, the accurate MS/MS data acquired through data-dependent analysis mode in another run facilitated the structural elucidations of degradation products. As a result, a total of 11 degradation products of danofloxacin were detected and characterized using the developed method. Overall, this analytical strategy enables the acquisition of accurate-mass LC/MS data, search of a variety of degradation products through the post-acquisition processes, and effective structural characterization based on elemental compositions of degradation product molecules and their product ions. The ability to measure degradation products via tandem mass spectrometry coupled with accurate mass measurement, all in only two experimental runs, is one of the most attractive features of this methodology. The results demonstrate that use of the LC/MS-IT-TOF approach appears to be rapid, efficient and reliable in structural characterization of drug degradation products.
authors.affiliation: Hunan Engineering Research Center of Veterinary Drugs, College of Veterinary Medicine, Hunan Agricultural University, Changsha, China.
authors.forename: Zhao-Ying
authors.initials: ZY
authors.lastname: Liu
authors.forename: Xiao-Ni
authors.initials: XN
authors.lastname: Zhou
authors.forename: Hua-Hai
authors.initials: HH
authors.lastname: Zhang
authors.forename: Leren
authors.initials: L
authors.lastname: Wan
authors.forename: Zhi-Liang
authors.initials: ZL
authors.lastname: Sun
mesh_terms: D000890:Anti-Infective Agents / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004355:Drug Stability; D024841:Fluoroquinolones / Q000737:chemistry*; D006868:Hydrolysis; D015394:Molecular Structure; D010084:Oxidation-Reduction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014466:Ultraviolet Rays
chemical_list: D000890:Anti-Infective Agents; D024841:Fluoroquinolones; C068581:danofloxacin