Usui Kiyotaka, Hayashizaki Yoshie, Hashiyada Masaki, Nakano Anri, Funayama Masato
Division of Forensic Medicine, Department of Public Health and Forensic Medicine, Tohoku University School of Medicine, Sendai 980-8575, Japan.
Leg Med (Tokyo). 2012 May;14(3):126-33. doi: 10.1016/j.legalmed.2012.01.006. Epub 2012 Feb 16.
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.
建立了一种液相色谱-串联质谱法,用于同时测定人血清和尿液样本中的四种乌头碱(乌头碱、新乌头碱、次乌头碱、杰斯乌头碱)及其七种水解产物(苯甲酰新乌头原碱、苯甲酰次乌头原碱、14-O-茴香酰乌头碱、苯甲酰乌头碱、乌头原碱、新乌头原碱、次乌头原碱)。采用混合型阳离子交换柱(OASIS MCX)进行萃取,以D(5)-乌头碱作为内标。使用L-column ODS对乌头生物碱进行分离,流动相由10mM甲酸铵和甲醇组成。日内和日间精密度分别为0.3%至9.9%和3.2%至12.8%。日内和日间准确度分别为-14.1%至7.3%和-10.6%至8.3%。分析物的检测限和定量限分别为0.04 - 0.38 ng/mL和0.12 - 1.15 ng/mL。该方法应用于一例尸检案例,成功检测到乌头碱及其代谢产物以及一些抗精神病药物。