Bulska Ewa, Bachliński Robert, Cyrański Michał K, Michalska-Kacymirow Magdalena, Kośnik Wioletta, Małecki Paweł, Grela Karol, Dobrowolski Michał A
Faculty of Chemistry, Biological and Chemical Research Center, University of Warsaw, Warsaw, Poland.
Central Forensic Laboratory of the Police, Warsaw, Poland.
Front Chem. 2020 Sep 25;8:693. doi: 10.3389/fchem.2020.00693. eCollection 2020.
A non-routine, comprehensive protocol for characterization of emerging new psychoactive substances (NPS) including chemical structures, impurities, as well as crystal structures, has been developed to facilitate the work of law enforcement agencies. A set of NPS has been synthesized, identified, and characterized by various analytical methods in order to be used as certified reference standards (CRMs). Seven selected compounds (5-IT, NM-2201, MT-45, AB-CHMINACA, UR-144, 5F-PB-22, and 4-CMC) were synthesized on the laboratory scale, then the process was upscaled to semi-technical. All products were analyzed by electrospray Q/TOF-MS/MS for molecular structure identification. The presence of by-products, as well as metal impurities, arising from the performed syntheses, were characterized by reversed phase liquid chromatography (RP-HPLC) with DAD and Q/TOF-MS detection and inductively-coupled plasma with quadrupole mass spectrometer (ICP-QMS), respectively. Additionally, the crystal structures of UR-144, NM-2201, 5F-PB-22, and 4-CMC have been determined by single-crystal and powder X-ray diffraction.
已制定了一项非常规的综合方案，用于鉴定新兴新型精神活性物质（NPS），包括化学结构、杂质以及晶体结构，以协助执法机构开展工作。已合成了一组NPS，并通过各种分析方法对其进行了鉴定和表征，以便用作认证参考标准物质（CRM）。在实验室规模上合成了七种选定的化合物（5-IT、NM-2201、MT-45、AB-CHMINACA、UR-144、5F-PB-22和4-CMC），然后将该过程扩大到半工业规模。所有产品均通过电喷雾Q/TOF-MS/MS进行分析以鉴定分子结构。分别通过带有二极管阵列检测器（DAD）和Q/TOF-MS检测的反相液相色谱（RP-HPLC）以及带有四极杆质谱仪的电感耦合等离子体（ICP-QMS）对合成过程中产生的副产物以及金属杂质的存在情况进行了表征。此外，已通过单晶和粉末X射线衍射确定了UR-144、NM-2201、5F-PB-22和4-CMC的晶体结构。
