Synthesis, characterisation and quantification of the new psychoactive substance 1-(1,3-benzodioxol-5-yl)-2-(propylamino)butan-1-one (bk-PBDB, putylone)

IF 2.6 3区 医学 Q2 CHEMISTRY, ANALYTICAL
David I. Dixon , Molly F. Millea , Alexander T. M. Wilcock , Andrew Costello , Jamie R. Ellison , Sacha Lord , Kim A. O'Brian , Ryan E. Mewis , Oliver B. Sutcliffe
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Abstract

Synthetic cathinones are a continually evolving family of illicit drugs, with novel analogues frequently being detected. This paper reports the detection of 1-(1,3-benzodioxol-5-yl)-2-(propylamino)butan-1-one, bk-PBDB (putylone), within solid dosage forms (tablets) seized by law enforcement for the first time in the United Kingdom. The identity of the compound was confirmed via the synthesis of a pure bk-PBDB reference standard and direct spectral comparison by 1H NMR and GC-EI-MS analysis. A full analytical profiling of bk-PBDB by nuclear magnetic resonance (NMR), attenuated total reflection Fourier-transform infrared (FTIR) spectroscopy and gas chromatography-electron ionisation-mass spectrometry (GC-EI-MS) is reported and shows good concordance between the seized sample and the reference standard. A validated GC-EI-MS method for the routine quantification of the cathinone in bulk forensic samples (LOD: 0.09 μg/mL, LOQ: 0.26 μg/mL) was also developed and using this method, the seized tablets were determined to contain a mixture of bk-PBDB (130.6–135.5 mg/tablet) and caffeine (40.2–43.4 mg/tablet) respectively.

Abstract Image

新型精神活性物质1-(1,3-苯并二氧唑-5-基)-2-(丙氨基)丁-1-酮(bk-PBDB,putylone)的合成、表征和定量
合成卡西酮是一个不断发展的非法药物家族,经常发现新的类似物。本文报道了英国执法部门首次在固体剂型(片剂)中检出1-(1,3-苯二酚-5-基)-2-(丙胺)丁酮-1- 1,bk-PBDB (putylone)。通过合成纯bk-PBDB标准品,并通过1H NMR和GC-EI-MS直接进行光谱比较,证实了该化合物的性质。利用核磁共振(NMR)、衰减全反射傅立叶变换红外(FTIR)光谱和气相色谱-电子电离-质谱(GC-EI-MS)对bk-PBDB进行了全面分析,结果表明,检获的样品与参比标准品具有良好的一致性。建立了法医学原料药中卡西酮(LOD: 0.09 μg/mL, LOQ: 0.26 μg/mL)常规定量的气相色谱-气相色谱-质谱联用方法,测定了检出的片剂中分别含有bk-PBDB (130.6 ~ 135.5 mg/片)和咖啡因(40.2 ~ 43.4 mg/片)。
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来源期刊
Forensic Chemistry
Forensic Chemistry CHEMISTRY, ANALYTICAL-
CiteScore
5.70
自引率
14.80%
发文量
65
审稿时长
46 days
期刊介绍: Forensic Chemistry publishes high quality manuscripts focusing on the theory, research and application of any chemical science to forensic analysis. The scope of the journal includes fundamental advancements that result in a better understanding of the evidentiary significance derived from the physical and chemical analysis of materials. The scope of Forensic Chemistry will also include the application and or development of any molecular and atomic spectrochemical technique, electrochemical techniques, sensors, surface characterization techniques, mass spectrometry, nuclear magnetic resonance, chemometrics and statistics, and separation sciences (e.g. chromatography) that provide insight into the forensic analysis of materials. Evidential topics of interest to the journal include, but are not limited to, fingerprint analysis, drug analysis, ignitable liquid residue analysis, explosives detection and analysis, the characterization and comparison of trace evidence (glass, fibers, paints and polymers, tapes, soils and other materials), ink and paper analysis, gunshot residue analysis, synthetic pathways for drugs, toxicology and the analysis and chemistry associated with the components of fingermarks. The journal is particularly interested in receiving manuscripts that report advances in the forensic interpretation of chemical evidence. Technology Readiness Level: When submitting an article to Forensic Chemistry, all authors will be asked to self-assign a Technology Readiness Level (TRL) to their article. The purpose of the TRL system is to help readers understand the level of maturity of an idea or method, to help track the evolution of readiness of a given technique or method, and to help filter published articles by the expected ease of implementation in an operation setting within a crime lab.
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