title: Identification and characterization of stressed degradation products of prulifloxacin using LC-ESI-MS/Q-TOF, MSn experiments: development of a validated specific stability-indicating LC-MS method.
abstract: A rapid, specific and novel gradient LC-MS method has been developed and validated for the identification and characterization of stressed degradation products (DPs) of prulifloxacin (PF) using liquid chromatography combined with quadrupole time-of-flight electrospray ionization tandem mass spectrometry (LC/Q-TOF-ESI-MS/MS). PF was subjected to hydrolytic (acidic, alkaline and neutral), oxidation, photolytic and thermal stress, as per ICH guidelines Q1A (R2). The drug showed extensive degradation in hydrolytic and oxidative, while it was stable to thermal and photolytic stress conditions. In total, 13 DPs were formed and the chromatographic separation of drug and its DPs was achieved on a C-18 column (4.6 × 250 mm, 5 μm) using gradient elution method. All the DPs have been identified and characterized using MS(n) experiments and accurate mass measurements. The LC-MS method was validated with respect to specificity, linearity, accuracy, precision and robustness.
authors.affiliation: National Centre for Mass Spectrometry, Indian Institute of Chemical Technology, Hyderabad 500 607, India.
authors.forename: B
authors.initials: B
authors.lastname: Raju
authors.forename: M
authors.initials: M
authors.lastname: Ramesh
authors.forename: R
authors.initials: R
authors.lastname: Srinivas
authors.forename: S Satyanarayana
authors.initials: SS
authors.lastname: Raju
authors.forename: Y
authors.initials: Y
authors.lastname: Venkateswarlu
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004148:Dioxolanes / Q000737:chemistry*; D004355:Drug Stability; D024841:Fluoroquinolones / Q000737:chemistry*; D006868:Hydrolysis; D010084:Oxidation-Reduction; D010782:Photolysis; D010879:Piperazines / Q000737:chemistry*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013678:Technology, Pharmaceutical / Q000379:methods*; D013696:Temperature
chemical_list: D004148:Dioxolanes; D024841:Fluoroquinolones; D010879:Piperazines; C074191:prulifloxacin