title: Isolation and characterization of a new human urinary metabolite of diclofenac applying LC-NMR-MS and high-resolution mass analyses.
abstract: The nonsteroidal anti-inflammatory drug diclofenac is widely used. Diclofenac is extensively metabolized to several hydroxylated derivatives and their conjugates. The lactam-dehydrate of 4'-hydroxy diclofenac (4'-OHDD) has now been detected as a new urinary metabolite of diclofenac. Isolation was successfully performed using preparative HPLC in three different steps using water, methanol, and acetonitrile, respectively. The structural characterization of 4'-OHDD was achieved by LC-NMR-MS. In addition, specific mass fragmentation pattern could be obtained using LC-high-resolution MS with both positive and negative electrospray ionization.
authors.affiliation: Institute of Environmental Research (INFU), University of Dortmund, Dortmund, Germany.
authors.forename: Dele
authors.initials: D
authors.lastname: Stülten
authors.forename: Marc
authors.initials: M
authors.lastname: Lamshöft
authors.forename: Sebastian
authors.initials: S
authors.lastname: Zühlke
authors.forename: Michael
authors.initials: M
authors.lastname: Spiteller
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis* / Q000737:chemistry / Q000652:urine; D002853:Chromatography, Liquid / Q000379:methods*; D004008:Diclofenac / Q000032:analysis* / Q000737:chemistry / Q000652:urine; D006801:Humans; D013058:Mass Spectrometry / Q000379:methods*; D015394:Molecular Structure; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*
chemical_list: D000894:Anti-Inflammatory Agents, Non-Steroidal; D004008:Diclofenac