Determination of 10α‐methoxy‐9,10‐dihydrolysergol, a nicergoline metabolite, in human urine by high performance liquid chromatography

A specific method for the determination of 10α‐methoxy‐9,10‐dihydrolysergol, a nicergoline metabolite (metabolite 2), in urine is described. Metabolite 2 was well separated from the urine components on a reversed phase column, Hypersil ODS 5 μm, using an acetonitrile: pH 3.5 phosphate buffer (40:60, v/v) as the mobile phase at a flow rate of 1 mL/min. UV detection was set up at 220 nm. After addition of a known amount of lysergamide as the internal standard, the compounds were extracted from alkalysed urine on a pre‐packed glass column (Extrelut 1) with dichloromethane. With 0.5 mL urine, concentrations down to 0.56 μmol/L could be determined.