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采用液相色谱-串联质谱法同时测定人血清和尿液中的11种乌头生物碱。

Simultaneous determination of 11 aconitum alkaloids in human serum and urine using liquid chromatography-tandem mass spectrometry.

作者信息

Usui Kiyotaka, Hayashizaki Yoshie, Hashiyada Masaki, Nakano Anri, Funayama Masato

机构信息

Division of Forensic Medicine, Department of Public Health and Forensic Medicine, Tohoku University School of Medicine, Sendai 980-8575, Japan.

出版信息

Leg Med (Tokyo). 2012 May;14(3):126-33. doi: 10.1016/j.legalmed.2012.01.006. Epub 2012 Feb 16.

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.

摘要

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。

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