Institute of Forensic Medicine, Forensic Toxicology, Johannes Gutenberg University Mainz, Mainz, Germany.
Drug Test Anal. 2021 Aug;13(8):1535-1551. doi: 10.1002/dta.3052. Epub 2021 May 5.
Analysis of synthetic cannabinoids still poses a challenge for many institutions due to the number of available substances and the constantly changing drug market. Both new and well-known substances keep appearing and disappearing on the market, making it hard to adapt analytical methods in a timely manner. In this study, we developed a qualitative screening approach for synthetic cannabinoids and their metabolites by means of liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). Samples were measured in data-dependent auto-MS/MS mode and identified by fragment spectra, retention time and accurate mass. Two established solid phase extractions were compared using fortified serum and urine samples. Mixes of 199 synthetic cannabinoids and 110 metabolites were used in 1- and 10-ng/ml concentrations. Up to 93% of synthetic cannabinoids and 74% of metabolites were detected in fortified 1-ng/ml samples. From February 2018 to October 2020, we analyzed 1492 cases, of which 73 cases were positive for synthetic cannabinoids or metabolites. 5F-MDMB-PICA, 4F-MDMB-BINACA, MDMB-4en-PINACA, and 4F-MDMB-BICA were most frequently detected. Hydrolysis metabolites were detected in many blood samples, providing a longer detection window. Quantification was conducted via liquid chromatography triple quadrupole mass spectrometry after liquid-liquid extraction. Concentrations were mostly close to 1 ng/ml in blood samples. LC-QTOF-MS was able to detect substances above trace quantities (< 0.1 ng/ml) in most cases, therefore fulfilling its purpose as a sensitive general screening approach. Expansion of the screening library was uncomplicated and enables future additions for up to thousands of targets.
由于可用物质的数量众多，以及毒品市场不断变化，许多机构在分析合成大麻素方面仍然面临挑战。新的和广为人知的物质不断出现在市场上并消失，使得及时调整分析方法变得困难。在这项研究中，我们通过液相色谱四极杆飞行时间质谱（LC-QTOF-MS）开发了一种用于合成大麻素及其代谢物的定性筛选方法。样品在数据依赖自动 MS/MS 模式下进行测量，并通过碎片图谱、保留时间和精确质量进行鉴定。使用加标血清和尿液样本比较了两种已建立的固相萃取方法。在 1-和 10-ng/ml 浓度下，使用了 199 种合成大麻素和 110 种代谢物的混合物。在加标 1-ng/ml 样品中，高达 93%的合成大麻素和 74%的代谢物被检测到。从 2018 年 2 月到 2020 年 10 月，我们分析了 1492 例病例，其中 73 例为合成大麻素或代谢物阳性。5F-MDMB-PICA、4F-MDMB-BINACA、MDMB-4en-PINACA 和 4F-MDMB-BICA 是最常检测到的物质。在许多血液样本中检测到水解代谢物，提供了更长的检测窗口。经液液萃取后，通过液相色谱三重四极杆质谱进行定量。血样中的浓度大多接近 1ng/ml。LC-QTOF-MS 能够在大多数情况下检测到痕量（<0.1ng/ml）以下的物质，因此作为一种敏感的通用筛选方法达到了其目的。筛选库的扩展并不复杂，并能够为未来添加数千个目标提供支持。
