Degradation and Impurity Profiling of Some Active Pharmaceutical Ingredients

Abstract

The cumulative objectives of present research work were as follows: newline1. To develop and validate accurate, precise, reproducible and reliable stability newlineindicating assay method. newline2. To perform stress degradation of some drugs with stability indicating assay method newlineas per ICH guidelines. newline3. To establish the structure of the degradants and degradation pathways of the drug newlinecandidates. newline4. To establish impurity profiling of some active pharmaceuticals (API) newlineFive APIs, viz. armodafinil (AMD), artemether (ART), olopatadine hydrochloride (OLO), newlineramelteon (RMT) and tapentadol hydrochloride (TAP) were used for the research work to newlineexplore the above objectives. newlineThe whole work was carried out on HPLC chromatograph model Agilent Infinity 1260 newlineseries equipped with 1260 binary pump VL 400 bar, 1260 manual injector 600 bar, newlineRheodyne 7725i 7-port sample injection valve with 20 and#956;L fixed loop, ZORBAX Eclipse newlinePlus C18 (250 × 4.6 mm, 5 and#61549;m), 1260 DAD VL, 20 Hz detector, standard flow cell 10 newlinemm, 13 and#61549;L, 120 bar, OpenLab CDS EZChrom Ed. Workstation and syringe 50.0 and#61549;L, FN, newlineLC tip. LC-MS was Micromass Q-TOF micro (Waters) equipped with separation module - newlineWaters Alliance 2795; LC column: Zorbax Eclipse Plus C18 column (250 × 4.6 mm, 5 newlineand#956;m); ionization - electro spray positive (ES+); acquisition: MRM (unit resolution). LC-MS newlinestudy was performed in positive mode using leucine enkephalin as standard. Ultraviolet newlinespectrophotometers (Shimadzu 1700 and 1800 series) with 1 cm matched quartz cells were newlineused for the present research work. newlineAs per ICH guidelines, developed methods for drugs were validated. The validated RPHPLC newlinemethods for APIs were successfully applied to establish degradation profiles and newlinestability indicating power of the method, as drugs were determined in presence of newlinedegradation products by their respective method. newline