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

• Published in: Forensic chemistry 2023-09, Vol.35, p.100523, Article 100523
• Main Authors: Dixon, David I., Millea, Molly F., M. Wilcock, Alexander T., Costello, Andrew, Ellison, Jamie R., Lord, Sacha, O'Brian, Kim A., Mewis, Ryan E., Sutcliffe, Oliver B.
• Format: Article
• Language: English
• Subjects: bk-PBDB; GC-EI-MS; NMR; Novel psychoactive substances; Synthetic cathinones
• ISSN: 2468-1709; 2468-1709
• DOI: 10.1016/j.forc.2023.100523

[Display omitted] •Novel synthetic cathinone bk-PBDB was detected in a seized solid dosage form.•Synthesis of bk-PBDB reference standard for comparison.•Full NMR, ATR-FTIR and GC-EI-MS characterisation of bk-PBDB is reported.•Development and validation of GC-EI-MS method of quantification.•Seized samples were determined by GC-EI-MS to contain a combination of bk-PBDB (130.6–135.5 mg/tablet) and caffeine (40.2–43.4 mg/tablet). 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.