A highly sensitive UHPLC-MS/MS method for determining 15 designer LSD analogs in biological samples with application to stability studies†

IF 3.6 3区 化学 Q2 CHEMISTRY, ANALYTICAL
Analyst Pub Date : 2024-12-05 DOI:10.1039/D4AN01361A
Olga Wachełko, Karolina Nowak, Kaja Tusiewicz, Marcin Zawadzki and Paweł Szpot
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Abstract

In recent years, the rise in the synthesis and distribution of LSD analogs in illicit drug markets, commonly referred to as “designer psychedelics”, has contributed to increased recreational use. This trend has resulted in a rising number of global reports, with law enforcement increasingly detecting these compounds in blotter papers and biological samples. In the presented paper, an UHPLC-QqQ-MS/MS method was developed for trace determination (fg mL−1) of LSD, its designer analogs (ALD-52, AL-LAD, LAMPA, LSM-775, LSZ, MiPLA, 1B-LSD, 1cP-LSD, 1cP-MiPLA, 1P-LSD, 1P-MiPLA, 1V-LSD and 2-Bromo-LSD) and its metabolite (2-oxo-3-OH-LSD) with simultaneous separation of structural isomers. Biological samples were prepared using liquid–liquid extraction (LLE) at pH 9 (with ethyl acetate); quantification was performed in multiple reaction monitoring (MRM) mode. LSD-d3 was used as an internal standard. The limit of quantification (LOQ) for all substances was 0.5 pg mL−1. Precision and accuracy did not exceed 15.8% and ±14.4%, respectively. Recovery and matrix effect values were 80.6–118.6% and ±19.4%. A stability study was conducted over 30 days under different storage conditions (25 °C, 4 °C and −20 °C) for blood, urine, plasma, and serum, collected in various test tube configurations and with different preservative agents. It was found that the collection of samples in NaF can effectively stabilize LSD analogs and minimize the conversion of N1-substituted compounds to LSD or MiPLA. The presented method is the most sensitive to date for analyzing designer LSD analogs in biological samples, with potential for routine clinical and forensic use, enhancing detection of emerging illicit compounds. By examining the mass spectra (QTOF-MS/MS) obtained in this study and reviewing the literature on analytical characterization of LSD analogs, we proposed fragmentation patterns to aid in future identification of new designer LSD analogs (NPS).

Abstract Image

Abstract Image

高效液相色谱-质谱联用法测定生物样品中15种设计剂LSD类似物,并应用于稳定性研究
近年来,非法药物市场上LSD类似物(通常称为“设计迷幻药”)的合成和分销增加,导致娱乐性使用增加。这一趋势导致全球报告数量不断增加,执法部门越来越多地在吸墨纸和生物样本中检测到这些化合物。本文建立了一种同时分离结构异构体的UHPLC-QqQ-MS/MS法测定LSD及其设计物ALD-52、AL-LAD、LAMPA、LSM-775、LSZ、MiPLA、1B-LSD、1cP-LSD、1cP-MiPLA、1P-LSD、1V-LSD和2-Bromo-LSD及其代谢产物2-oxo-3-OH-LSD的痕量(fg mL−1)。生物样品采用液液萃取法(LLE)制备,pH为9(乙酸乙酯);采用多反应监测(MRM)模式进行定量。内标为LSD-d3。所有物质的定量限(LOQ)为0.5 pg mL−1。精密度和准确度分别不超过15.8%和±14.4%。回收率为80.6 ~ 118.6%,基质效应值为±19.4%。在不同的保存条件(25°C、4°C和- 20°C)下,对血液、尿液、血浆和血清进行了为期30天的稳定性研究,这些血液、尿液、血浆和血清采集于不同的试管配置和不同的防腐剂中。研究发现,在NaF中收集样品可以有效地稳定LSD类似物,并最大限度地减少n1取代化合物向LSD或MiPLA的转化。该方法是迄今为止分析生物样品中设计LSD类似物最敏感的方法,具有常规临床和法医应用的潜力,增强了对新出现的非法化合物的检测。通过分析本研究获得的质谱(QTOF-MS/MS)和回顾LSD类似物分析表征的文献,我们提出了碎片模式,以帮助未来鉴定新的设计LSD类似物(NPS)。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
Analyst
Analyst 化学-分析化学
CiteScore
7.80
自引率
4.80%
发文量
636
审稿时长
1.9 months
期刊介绍: "Analyst" journal is the home of premier fundamental discoveries, inventions and applications in the analytical and bioanalytical sciences.
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