1H quantitative NMR and UHPLC-MS analysis of seized MDMA/NPS mixtures and tablets from night-club venues

Husain A Naqi,Ian S Blagbrough,Stephen M Husbands

doi:10.1039/c9ay01403a

Husain A Naqi, Ian S Blagbrough + Show 1 more

Open Access

https://doi.org/10.1039/c9ay01403a

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Abstract

A fast (15 min), accurate and reproducible 1H q-NMR (in D2O) analysis performed on many samples containing complex mixtures of MDMA and NPS revealing significant differences in their ratios.

Highlights

3,4-Methylenedioxymethamphetamine (MDMA) in the UK has increased in purity and the contents sold as MDMA have increased in complexity
Seized MDMA tablets were quanti ed using 1H quantitative NMR (q-NMR) and crossmethod con rmed using UHPLC equipped with a variable wavelength detector (VWD) and UHPLC-MS using MDMA-d5 as an internal standard (IS)
Where x is the analyte, std is the IS, m is the mass in mg, P is the purity, Mw is the molecular weight in g molÀ1, A is the integral value of the resonance being investigated, N is the number of protons represented by the signal, m(sample) is the mass of the sample/tablet in mg and m(sample used) is the mass of the extracted sample, e.g. 10.00 mg. 1H q-NMR of MDMA/methylone/tri uoromethylpiperazine (TFMPP) and MDMA/ethylone mixtures using maleic acid (MA) as an IS resonating at d 1⁄4 6.38 ppm was performed

Summary

Analytical Methods

HPLC and GC are the gold standard analytical methods in forensic laboratories for the quantification of seized samples of illicit drugs. A 1H quantitative NMR (q-NMR) method is developed for the quantification of seized samples from night-clubs. These samples are shown to contain mixtures of MDMA and other NPS, e.g. ethylone, methylone, trifluoromethylpiperazine (TFMPP), N,N-dimethyl-3,4methylenedioxyamphetamine (MDDMA), 4-bromo-2,5-dimethoxyphenethylamine (2C-B), and 4-iodo2,5-dimethoxyphenethylamine (2C-I). 1H q-NMR provides a fast (15 min) and robust analytical method for the quantification of complex seized samples without resorting to tedious sample preparation or obtaining reference standards The method is applied to MDMA tablets seized from similar venues, and compared with UHPLC and UHPLC-MS, resulting in a good agreement across techniques. 1H q-NMR provides a fast (15 min) and robust analytical method for the quantification of complex seized samples without resorting to tedious sample preparation or obtaining reference standards

Introduction

Results and discussion

Conclusions

25 European Network of Forensic Science Institutes – Drugs