title: Validation of a reversed-phase HPLC method for 1,10-phenanthroline-5,6-dione and analysis of its impurities by HPLC-MS.
abstract: A reversed-phase HPLC analytical method for the assay of 1,10-phenanthroline-5,6-dione (I) has been developed and validated. A C18 column (150 x 4.6 mm; 5 microm) was employed together with a mobile phase of methanol-water (50:50, v/v) containing 0.1% triethylamine. UV detection was performed at 254 nm. Dione (I) eluted as a spectrally pure peak resolved from its impurities allowing the method to be applied to the purity evaluation of samples obtained via two synthetic routes. In addition, 4,5-diazafluoren-9-one (V) was identified as the main impurity by employing the method in HPLC-MS mode with photodiode array UV detection.
authors.affiliation: Abbott Laboratories, MediSense UK Ltd., 14/15 Eyston Way, Abingdon, Oxon OX14 1TR, UK.
authors.forename: Ghulam A
authors.initials: GA
authors.lastname: Shabir
authors.forename: Nigel J
authors.initials: NJ
authors.lastname: Forrow
mesh_terms: D000970:Antineoplastic Agents / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D004340:Drug Contamination; D004355:Drug Stability; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D019999:Pharmaceutical Solutions; D010618:Phenanthrolines / Q000032:analysis* / Q000138:chemical synthesis; D011809:Quinones / Q000032:analysis; D012015:Reference Standards; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet
chemical_list: D000970:Antineoplastic Agents; D007202:Indicators and Reagents; D019999:Pharmaceutical Solutions; D010618:Phenanthrolines; D011809:Quinones; C037153:1,10-phenanthroline-5,6-dione