School of Pharmacy and Biomolecular Sciences, Liverpool John Moores University, Liverpool, UK.
School of Chemical Engineers, University of Upper Alsace, Mulhouse, France.
Drug Test Anal. 2020 Aug;12(8):1109-1125. doi: 10.1002/dta.2813. Epub 2020 Jun 10.
Two groups of amphetamine-like drugs with psychostimulant properties that were first developed during the course of scientific studies and later emerged as new psychoactive substances (NPS) are based on the (2-aminopropyl)indole (API) and (2-aminopropyl)benzofuran (APB) structural scaffolds. However, sulfur-based analogs with a benzo[b]thiophene structure (resulting in (2-aminopropyl)benzo[b]thiophene (APBT) derivatives) have received little attention. In the present investigation, all six racemic APBT positional isomers were synthesized in an effort to understand their structure-activity relationships relative to API- and APB-based drugs. One lesson learned from the NPS phenomenon is that one cannot exclude the appearance of such substances on the market. Therefore, an in-depth analytical characterization was performed, including various single- and tandem mass spectrometry (MS) and ionization platforms coupled to gas chromatography (GC) and liquid chromatography (LC), nuclear magnetic resonance spectroscopy (NMR), and solid phase and GC condensed phase infrared spectroscopy (GC-sIR). Various derivatizations have also been explored; it was found that all six APBT isomers could be differentiated during GC analysis after derivatization with heptafluorobutyric anhydride and ethyl chloroformate (or heptafluorobutyric anhydride and acetic anhydride) under non-routine conditions. Discriminating analytical features can also be derived from NMR, GC-EI/CI- single- and tandem mass spectrometry, LC (pentafluorophenyl stationary phase), and various infrared spectroscopy approaches (including GC-sIR). Availability of detailed analytical data obtained from these novel APBT-type stimulants may be useful to researchers and scientists in cases where forensic and clinical investigations are warranted.
两组具有精神兴奋特性的苯丙胺类药物最初是在科学研究过程中开发的,后来作为新的精神活性物质(NPS)出现,它们基于(2-氨基丙基)吲哚(API)和(2-氨基丙基)苯并呋喃(APB)结构支架。然而,基于苯并[b]噻吩结构的含硫类似物(导致(2-氨基丙基)苯并[b]噻吩(APBT)衍生物)受到的关注较少。在本研究中,合成了所有六种外消旋 APBT 位置异构体,以了解它们与基于 API 和 APB 的药物的结构-活性关系。从 NPS 现象中得到的一个教训是,不能排除此类物质出现在市场上。因此,进行了深入的分析表征,包括各种单和串联质谱(MS)和电离平台与气相色谱(GC)和液相色谱(LC)、核磁共振波谱(NMR)以及固相和 GC 凝聚相红外光谱(GC-sIR)的结合。还探索了各种衍生化方法;发现所有六种 APBT 异构体在衍生化后均可用 GC 分析进行区分,衍生化条件为七氟丁酰酐和氯甲酸乙酯(或七氟丁酰酐和乙酸酐)在非常规条件下。NMR、GC-EI/CI-单和串联质谱、LC(五氟苯基固定相)和各种红外光谱方法(包括 GC-sIR)也可以得出有区别的分析特征。获得的这些新型 APBT 型兴奋剂的详细分析数据可能对需要进行法医和临床调查的研究人员和科学家有用。