Increasing amounts of new psychoactive substances (NPS) are being developed every year under non-regulated conditions. A major concern is that such substances can be bought legally by consumers, which not only poses unknown health risks, but also represents a significant challenge to both medical and law enforcement personnel.
Illegal and legal substances such as regioisomers can share very similar structures, meaning the analytical information used to test drugs should be able to accurately discern between them.
This article demonstrates the importance of nuclear magnetic resonance (NMR) in identifying the exact structure of legal and illegal drugs.
It is demonstrated here how DOSY experiments can be performed in combination with computer-assisted structure verification of the different compounds that are found in artificial drugs such as China White.
In addition, the article demonstrates how the structural data acquired can be utilized to streamline the detection and quantification of compounds found in recreational drugs using matching tools and library search.
The NPS detected for the first time in the current year, as well as those detected in previous years are shown in Figure 1.
Figure 1. NPS identified from year 2009 to 2013
Results and Discussion
Ketamine - Confirming Regio-isomerism
NMR was performed to examine a ketamine sample in order to confirm the structure (class B compound) and rule out regioisomers (non-classified). Using CMC-se software, including long-range HC correlations, this verification was achieved.
Figure 2 shows the new structure drawing tool used for the process.
Figure 2. The use of the new structure drawing tool for verification in CMC-se China White
The isolation of compounds (A and B) using DOSY is illustrated in Figure 3, and Figures 3a to 3c show the elucidation of A using CMC-se. The same procedure was performed for compound B, which was identified as benzocaine.
Figure 3. Mixture analysis workflow
The NMR spectra and the structure for methiopropamine and benzocaine were introduced into a database. A technique was designed that would identify and quantify these compounds in mixtures using Assure Raw Material Screening (Assure RMS), a process that can be completely automated from acquisition through to report generation (Figure 4).
By using the new Assure RMS technique, additional analysis of China White batches can be conducted simply at the touch of a button, therefore significantly reducing the analysis time.
Figure 4. Identification and quantification with Assure RMS
NMR is an important technique in the analysis of NPS. The use of CMC-se software for this analysis provides several advantages such as structural verification, clarification of NPS from scratch, and discrimination between regioisomers. In addition, the software removes bias and tunnel effect and enables complete investigation of the entire chemical space.
The NPS mixture analysis workflow involved CMC-se of a single compound at a time; DOSY for separating compounds and Assure RMS for the identification, databasing, and quantification of compounds.
 ‘Global Synthetic Drugs Assessment’ report, UNODC, http://www.unodc.org/documents/southeastasiaandpacific/2014/05/gsda/2014_Global_Synthetic_Drugs_Assessment_embargoed_Tokyo_web.pdf, accessed 18 Dec 14,
 http://www.bruker.com/products/mr/nmr/nmr-software/software/complete-molecular-confidence/cmc-se/overview.html, accessed 18 Dec 14
 http://www.bruker.com/products/mr/nmr/nmr-software/software/assure/overview.html, accessed 18 Dec 14
Produced from materials authored by Anna Codina1, Peter Gierth1, Chris Stapleton1, Andrew Kirkham1, Julia Smith1, Nicola Tonge1, Nora Kouris1, Brian Marquez2, Andrew Gibbs1 and John Ramsey3.
1Bruker UK Limited, Banner Lane, Coventry, CV4 9GH, UK
2Bruker BioSpin, 15 Fortune Drive, Billerica MA 01821, USA
3TICTAC Communications Ltd.
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