LC-MS analysis of human urine specimens for 2-oxo-3-hydroxy LSD: Method validation for potential interferants, and stability study of 2-oxo-3-hydroxy LSD under various storage conditions
LC-MS analysis of human urine specimens for 2-oxo-3-hydroxy LSD: Method validation for potential interferants, and stability study of 2-oxo-3-hydroxy LSD under various storage conditions
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DOI：
10.1093/jat/26.4.193
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发表时间：
2002-05-01
影响因子：
2.5
通讯作者：
Anderson, CJ
中科院分区：
文献类型：
--
作者：
Klette, KL;Horn, CK;Anderson, CJ
2-氧代-3-羟基麦角酰二乙胺（O-H-LSD）是LSD的主要代谢产物，与母体药物LSD相比，已被证明是识别LSD使用的上级标志物。具体而言，据报道，使用液相色谱-质谱法分析的O-H-LSD在尿液中的浓度是LSD的16至43倍。为了进一步支持该程序的法医应用，使用具有与O-H-LSD相似的结构和化学性质的化合物评估了测定的特异性，这些化合物在非处方产品、处方药及其一些代谢物和其他滥用药物中常见。在研究的广泛化合物中，未发现干扰O-H-LSD或内标物2-氧代-3-羟基麦角酸甲基丙酰胺的检测。在不同温度、pH条件和暴露于荧光下研究了0 - 9天O-H-LSD的稳定性。此外，从0到60天，研究了长期冷冻储存和pH值的影响。在正常人体尿液生理pH范围内（4.6-8.4），冷藏和冷冻条件下O-H-LSD均无显著损失。然而，在pH 4.6-8.4下制备并在室温或更高温度（24-50°C）下储存的样品中观察到O-H-LSD的显著损失。
2-Oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD), a major LSD metabolite, has previously been demonstrated to be a superior marker for identifying LSD use compared with the parent drug, LSD. Specifically, O-H-LSD analyzed using liquid chromatography-mass spectrometry has been reported to be present in urine at concentrations 16 to 43 times greater than LSD. To further support forensic application of this procedure, the specificity of the assay was assessed using compounds that have structural and chemical properties similar to O-H-LSD, common over.the.counter products, prescription drugs and some of their metabolites, and other drugs of abuse. Of the wide range of compounds studied, none were found to interfere with the detection of O-H-LSD or the internal standard 2-oxo-3-hydroxy lysergic acid methyl propylamide. The stability of O-H-LSD was investigated from 0 to 9 days at various temperatures, pH conditions, and exposures to fluorescent light. Additionally, the effect of long-term frozen storage and pH was investigated from 0 to 60 days. There was no significant loss of O-H-LSD under both refrigerated and frozen conditions within the normal human physiological pH range of urine (4.6–8.4). However, significant loss of O-H-LSD was observed in samples prepared at pH 4.6–8.4 and stored at room temperature or higher (24–50°C).