title: Stress degradation studies on lornoxicam using LC, LC-MS/TOF and LC-MSn.
abstract: Lornoxicam was subjected to forced degradation studies under hydrolytic (acidic, basic and neutral), oxidative, photolytic and thermal stress conditions, as defined under ICH guideline Q1A (R2). The drug degraded significantly in hydrolytic, oxidative and photoneutral conditions, leading to the formation of eight degradation products in total. It was stable on exposure to light and dry heat in the solid state. The stressed samples in which degradation was observed were mixed together and used to develop a stability-indicating HPLC method wherein degradation products were separated from the drug and also from each other. To characterize the degradation products, a complete mass fragmentation pathway of the drug was first established with the help of MS/TOF, MS(n) and H/D exchange mass studies. The same was followed by LC-MS/TOF and on-line H/D exchange experiments on the degradation products. The degradation pathway of the drug was outlined, justified by the mechanisms of formation of the degradation products.
authors.affiliation: Department of Pharmaceutical Analysis, National Institute of Pharmaceutical Education and Research, Sector 67, SAS Nagar 160 062, Punjab, India.
authors.forename: Dattatray T
authors.initials: DT
authors.lastname: Modhave
authors.forename: Tarun
authors.initials: T
authors.lastname: Handa
authors.forename: Ravi P
authors.initials: RP
authors.lastname: Shah
authors.forename: Saranjit
authors.initials: S
authors.lastname: Singh
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D004355:Drug Stability; D006868:Hydrolysis; D013058:Mass Spectrometry / Q000379:methods*; D010084:Oxidation-Reduction; D010782:Photolysis; D010894:Piroxicam / Q000031:analogs & derivatives* / Q000737:chemistry; D013678:Technology, Pharmaceutical / Q000379:methods
chemical_list: D010894:Piroxicam; C059451:lornoxicam