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Münster-Müller, S.* ; Scheid, N.* ; Zimmermann, R. ; Pütz, M.*

Combination of stable isotope ratio data and chromatographic impurity signatures as a comprehensive concept for the profiling of highly prevalent synthetic cannabinoids and their precursors.

Anal. Chim. Acta 1108, 129-141 (2020)

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In this study, we utilized elemental analyser (EA) and gas-chromatography (GC) isotope ratio mass spectrometry (IRMS) and ultra-high-performance liquid chromatography coupled to mass spectrometry (UHPLC-MS) in a comprehensive profiling approach assessing the chromatographic impurity signatures and delta C-13 and delta(15) N isotope ratios of synthetic cannabinoids from police seizures and internet test purchases. Main target of this study was the highly prevalent synthetic cannabinoid MDMB-CHMICA (methyl(2S)-2-([1-(cyclohexylmethyl)- 1H-indol-3 -yl] formamido)-3 ,3-dimethylbutaoate). Overall, 61 powder and 118 herbal blend (also called "Spice-Products") samples were analysed using both analytical techniques and evaluated in a joint model to link samples from a common source. As a key finding, three agglomerates of Spice-product samples with similar dates of purchase were identified in the IRMS data, possibly representing larger shipments of MDMB-CHMICA, each produced with the same precursor material, successively delivered to the European market. The three agglomerates were refined into multiple sub-clusters based on the impurity profiling data, each representing an individual synthesis batch. One of the agglomerates identified in the IRMS data was found to consist two groups of four subclusters, respectively, with majorly different impurity profiles, demonstrating the necessity for both analytical techniques to extract the maximum amount of information from a limited sample pool. Additionally, 31 samples containing the recently surfaced synthetic cannabinoid Cumyl-PeGaClone (5pentyl-2-(2-phenylpropan-2-yl)-2,5-dihydro-1H-pyrido[4,3-blindol-1-one) were analysed for their and delta C-13 and delta N-15 isotope ratios to put the isotopic data recorded for MDMB-CHMNICA in a more global perspective. Three building blocks of precursor chemicals (indole, tert-leucine, cumylamine) potentially used for the synthesis of the two named synthetic cannabinoids were acquired from different global vendors and measured for their delta C-13 and delta N-15 isotope ratios to better understand variations in the isotopic composition of the synthetic cannabinoids and to trace their origin.

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