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Open Access Green möglich sobald Postprint bei der ZB eingereicht worden ist.
Impact of reaction parameters on the chemical profile of 3,4-methylenedioxymethamphetamine synthesized via reductive amination: Target analysis based on GC-qMS compared to non-targeted analysis based on GC×GC-TOF-MS.
Forensic Sci. Int. 223, 201-211 (2013)
The most common clandestine manufacturing procedure for the ecstasy derivative 3,4-methylenedioxymethamphetamine (MDMA), is the reductive amination of piperonylmethylketone (PMK) via platinum(IV) oxide/hydrogen. Deviations of the reaction conditions during the synthesis may result in different chemical profiles of the products. The chemical analysis of these profiles is an important objective for forensic drug intelligence. In this work we studied the impact of a systematic variation of the hydrogenation time, the reaction temperature and the precursor batch on the resulting organic chemical profiles of the MDMA bases and MDMA hydrochlorides. Target analysis was based on a gas chromatography mass spectrometry (GC-MS) method which was harmonized during the European project CHAMP.22Collaborative Harmonisation of Methods for Profiling of Amphetamine Type Stimulants. In addition, samples were analyzed by comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC. ×. GC-TOFMS) and subjected to non-targeted data analysis for a comprehensive analysis of the complete profiles. The reaction temperature, followed by the used precursor batch, revealed the highest impact on the chemical profile. The effect on individual impurity compounds is discussed in detail. With respect to the interpretation of the data, the profiles were compared to the profiles of MDMA samples obtained by reductive amination using sodium borohydride ("cold method") and aluminium/mercury amalgam as alternative reducing agents. Non-targeted analysis revealed that the discrimination according to the synthetic route and the batch of precursor used for the synthesis strongly depends on the selected target compounds.
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Publikationstyp
Artikel: Journalartikel
Dokumenttyp
Wissenschaftlicher Artikel
Schlagwörter
ATS; Comprehensive two-dimensional GC; Drug intelligence; Ecstasy; Impurity profiling; MDMA; Gas-chromatography ; Mdma Tablets ; Mass-spectrometry ; Organic Impurities ; Route ; Samples
ISSN (print) / ISBN
0379-0738
e-ISSN
1872-6283
Zeitschrift
Forensic Science International
Quellenangaben
Band: 223,
Heft: 1-3,
Seiten: 201-211
Verlag
Elsevier
Nichtpatentliteratur
Publikationen
Begutachtungsstatus
Peer reviewed