title: Simultaneous determination of 11 aconitum alkaloids in human serum and urine using liquid chromatography-tandem mass spectrometry.
abstract: A liquid chromatography-tandem mass spectrometry method was developed and validated for simultaneous determination of four aconitines (aconitine, mesaconitine, hypaconitine, jesaconitine) and seven of their hydrolysis products (benzoylmesaconine, benzoylhypaconine, 14-O-anisoylaconine, benzoylaconine, aconine, mesaconine, hypaconine) in human serum and urine samples. Extraction was undertaken using a mixed-mode cation-exchange cartridge (OASIS MCX), and D(5)-aconitine was used as an internal standard. Separation of aconitum alkaloids was carried out using an L-column ODS with the mobile phase consisting of 10mM ammonium formate and methanol. The intra- and inter-day precisions were 0.3% to 9.9% and 3.2% to 12.8%, respectively. Intra- and inter-day accuracies were -14.1% to 7.3%, and -10.6% to 8.3%, respectively. The limit of detection and limit of quantification of analytes were 0.04-0.38 ng/mL and 0.12-1.15 ng/mL respectively. This method was applied in an autopsy case and successfully detected aconitines and their metabolites as well as some anti-psychiatric drugs.
authors.affiliation: Division of Forensic Medicine, Department of Public Health and Forensic Medicine, Tohoku University School of Medicine, Sendai 980-8575, Japan. usui@forensic.med.tohoku.ac.jp
authors.forename: Kiyotaka
authors.initials: K
authors.lastname: Usui
authors.forename: Yoshie
authors.initials: Y
authors.lastname: Hayashizaki
authors.forename: Masaki
authors.initials: M
authors.lastname: Hashiyada
authors.forename: Anri
authors.initials: A
authors.lastname: Nakano
authors.forename: Masato
authors.initials: M
authors.lastname: Funayama
mesh_terms: D031841:Aconitum / Q000737:chemistry*; D000470:Alkaloids / Q000097:blood* / Q000652:urine*; D002853:Chromatography, Liquid; D006801:Humans; D007564:Japan; D053719:Tandem Mass Spectrometry
chemical_list: D000470:Alkaloids