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液相色谱-串联质谱法测定法医样本中的麦角酸二乙酰胺(LSD)、异麦角酸二乙酰胺(ISO-LSD)及其主要代谢物2-氧代-3-羟基-麦角酸二乙酰胺,并应用于一起法医案件

Liquid chromatography-tandem mass spectrometry determination of LSD, ISO-LSD, and the main metabolite 2-oxo-3-hydroxy-LSD in forensic samples and application in a forensic case.

作者信息

Johansen Sys Stybe, Jensen Jytte Lundsby

机构信息

Department of Forensic Chemistry, Institute of Forensic Medicine, University of Copenhagen, Frederik V's vej 11, DK-2100 Copenhagen Ø, Denmark.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Oct 15;825(1):21-8. doi: 10.1016/j.jchromb.2004.12.040. Epub 2005 Jan 26.

Abstract

A liquid chromatography mass spectrometric (LC/MS/MS) method has been developed for the determination of LSD, iso-LSD and the metabolite 2-oxo-3-hydroxy-LSD in forensic applications. The procedure involves liquid-liquid extraction of the analytes and LSD-D3 (internal standard) from 1.0 g whole blood or 1.0 ml urine with butyl acetate at pH 9.8. Confirmation and quantification were done by positive electrospray ionisation with a triple quadrupole mass spectrometer operating in multiple reaction monitoring (MRM) mode. Two MRM transitions of each compound were established and identification criteria were set up based on the retention time and the ion ratio. The curves of extracted standards were linear over a working range of 0.01-50 microg/kg for all transitions of LSD and iso-LSD. The limit of quantification was 0.01 microg/kg for LSD and iso-LSD. The method was applied to a case investigation involving a 26-year-old male suspected for having attempted homicide, where blood concentrations of LSD and iso-LSD were determined to 0.27 and 0.44 microg/kg, respectively. 2-Oxo-3-hydroxy-LSD was detected in the urine and confirmed the LSD abuse. The case illustrated the importance of analyte separation before MRM detection of a sample due to identical fragmentation ions of the isomers.

摘要

已开发出一种液相色谱质谱联用(LC/MS/MS)方法,用于法医应用中麦角酸二乙酰胺(LSD)、异麦角酸二乙酰胺(iso-LSD)及其代谢物2-氧代-3-羟基-LSD的测定。该程序包括用pH 9.8的乙酸丁酯从1.0 g全血或1.0 ml尿液中液液萃取分析物和LSD-D3(内标)。通过正电喷雾电离,使用在多反应监测(MRM)模式下运行的三重四极杆质谱仪进行确认和定量。确定了每种化合物的两个MRM转换,并根据保留时间和离子比率建立了鉴定标准。对于LSD和iso-LSD的所有转换,提取标准曲线在0.01-50微克/千克的工作范围内呈线性。LSD和iso-LSD的定量限均为0.01微克/千克。该方法应用于一起涉及一名涉嫌企图杀人的26岁男性的案件调查,其中LSD和iso-LSD的血药浓度分别测定为0.27和0.44微克/千克。在尿液中检测到2-氧代-3-羟基-LSD,证实了LSD滥用情况。该案例说明了由于异构体的碎片离子相同,在对样品进行MRM检测之前进行分析物分离的重要性。

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