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采用气相色谱-高分辨轨道阱质谱联用技术测定人尿液中的 5-MeO-DIPT

Determination of 5-MeO-DIPT in Human Urine Using Gas Chromatography Coupled with High-Resolution Orbitrap Mass Spectrometry.

机构信息

Department of Pharmaceutical Analysis, School of Pharmacy, Shenyang Pharmaceutical University, Wenhua Road 103, Shenyang 110016, China.

Department of Forensic Toxicology, Academy of Forensic Science, Shanghai Key laboratory of Forensic Medicine, 1347 West Guangfu Road, Shanghai 20063, China.

出版信息

J Anal Toxicol. 2020 Apr 2;44(5):461-469. doi: 10.1093/jat/bkaa005.

Abstract

5-Methoxy-N,N-Diisopropyltryptamine (5-MeO-DIPT) is a designer hallucinogen derived from tryptamine and its use has been banned by many countries. In this study, a qualitative and quantitative method was developed for determining 5-MeO-DIPT in urine by gas chromatography high-resolution mass spectrometry. 5-hydroxy-N,N-diisopropyltryptamine (5-OH-DIPT) and 5-methoxy-N-isopropyltryptamine (5-MeO-IPT) were identified as 5-MeO-DIPT metabolites in abusers' urine. 5-MeO-DIPT was extracted from urine by liquid-liquid extraction with ethyl acetate under alkaline conditions. The extract was analyzed by GC-Orbitrap-MS in full scan mode with a resolution of 60,000 full width at half maxima (FWHM). The linear range of this method was 2-300 ng/mL with r > 0.99, and the limit of detection was 1 ng/mL. The accuracy and precision were 93-108.7% and 3.1-10.3%, respectively. This method is simple and sensitive. It has been successfully used to detect 5-MeO-DIPT in drug abusers' urine, which showed that the concentrations of 5-MeO-DIPT were between 1 and 2.8 ng/mL. 5-OH-DIPT and 5-MeO-IPT, two urinary major metabolites of 5-MeO-DIPT, were identified in urine samples from 5-MeO-DIPT users. Furthermore, the stability of 5-MeO-DIPT in human urine was investigated. It was discovered that the concentration of 5-MeO-DIPT in urine decreased by 22.8, 33.2 and 38.2% after samples were stored for 24 h at 25°C, 5 days at 4°C and 7 days at 4°C, respectively. And 5-MeO-DIPT in urine were stable after they were stored for 30 days at -20°C. Therefore, it is recommended that urine should be stored under freezing conditions before performing 5-MeO-DIPT analysis.

摘要

5-甲氧基-N,N-二异丙基色胺(5-MeO-DIPT)是一种源自色胺的设计迷幻剂,许多国家已将其使用列为非法。在这项研究中,开发了一种通过气相色谱高分辨率质谱法定量和定性测定尿液中 5-MeO-DIPT 的方法。在滥用者的尿液中鉴定出 5-羟基-N,N-二异丙基色胺(5-OH-DIPT)和 5-甲氧基-N-异丙基色胺(5-MeO-IPT)为 5-MeO-DIPT 的代谢物。5-MeO-DIPT 是在碱性条件下用乙酸乙酯通过液液萃取从尿液中提取的。提取物在全扫描模式下通过 GC-Orbitrap-MS 进行分析,分辨率为 60,000 半峰全宽(FWHM)。该方法的线性范围为 2-300ng/mL,r>0.99,检测限为 1ng/mL。准确度和精密度分别为 93-108.7%和 3.1-10.3%。该方法简单灵敏。已成功用于检测药物滥用者尿液中的 5-MeO-DIPT,结果显示 5-MeO-DIPT 浓度在 1-2.8ng/mL 之间。在 5-MeO-DIPT 使用者的尿液样本中鉴定出 5-MeO-DIPT 的两种主要代谢物 5-OH-DIPT 和 5-MeO-IPT。此外,还研究了 5-MeO-DIPT 在人尿液中的稳定性。结果发现,尿液中 5-MeO-DIPT 的浓度在 25°C 下储存 24 小时、4°C 下储存 5 天和 4°C 下储存 7 天分别下降了 22.8%、33.2%和 38.2%。在-20°C 下储存 30 天后,尿液中的 5-MeO-DIPT 稳定。因此,建议在进行 5-MeO-DIPT 分析之前,将尿液储存在冷冻条件下。

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