Determination of LSD and its metabolites in human biological fluids by high-performance liquid chromatography with electrospray tandem mass spectrometry

J Canezin , A Cailleux , A Turcant , A Le Bouil , P Harry , P Allain
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引用次数: 53

Abstract

A liquid chromatographic procedure with electrospray ionization tandem mass spectrometric detection has been developed and validated for LSD and iso-LSD determination. A one-step liquid–liquid extraction on 1 ml blood or urine was used. The lower limit for quantitative determination was 0.02 μg/l for LSD and iso-LSD. The analytical procedure has been applied in two positive cases (case 1: LSD=0.31 μg/l, iso-LSD=0.27 μg/l in plasma and LSD=1.30 μg/l, iso-LSD=0.82 μg/l in urine; case 2: LSD=0.24 μg/l, iso-LSD=0.6 μg/l in urine). LSD metabolism was investigated using MS–MS neutral loss monitoring for the screening of potential metabolites. The main metabolite was 2-oxo-3-hydroxy-LSD (O–H–LSD) present in urine at the concentrations of 2.5 μg/l and 6.6 μg/l, respectively, for case 1 and 2, and was not present in plasma. Nor-LSD was also found in urine at 0.15 and 0.01 μg/l levels. Nor-iso-LSD, lysergic acid ethylamide (LAE), trioxylated-LSD, lysergic acid ethyl-2-hydroxyethylamide (LEO) and 13 and 14-hydroxy-LSD and their glucuronide conjugates were detected in urine using specific MS–MS transitions.

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高效液相色谱-电喷雾串联质谱法测定人体液中LSD及其代谢物
电喷雾电离串联质谱检测的液相色谱方法已经开发并验证了LSD和异LSD的测定。采用1 ml血液或尿液一步液-液萃取法。LSD和异LSD的定量下限为0.02 μg/l。本方法已应用于2例阳性病例(病例1:血浆中LSD=0.31 μg/l, iso-LSD=0.27 μg/l;尿液中LSD=1.30 μg/l, iso-LSD=0.82 μg/l;病例2:尿中LSD=0.24 μg/l, iso-LSD=0.6 μg/l)。采用MS-MS中性损失监测方法研究LSD代谢,筛选潜在代谢物。主要代谢物为2-氧-3-羟基lsd (O-H-LSD),在病例1和病例2中分别以2.5 μg/l和6.6 μg/l的浓度存在于尿液中,而在血浆中不存在。尿液中也发现了0.15和0.01 μg/l的非lsd。采用特异的质谱联用技术检测尿中非异异lsd、麦角酸乙基酰胺(LAE)、三氧化lsd、麦角酸乙基-2-羟乙基酰胺(LEO)、13和14-羟基lsd及其葡萄糖醛酸缀合物。
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