A Validated NMR Approach for MDMA Quantification in Ecstasy Tablets

Abstract

In recent years, ecstasy trafficking has grown in complexity and tablets has been commonly sold containing different contents of 3,4-methylenedioxymethamphetamine (MDMA) or even other psychoactive substances. In contrast, identification and quantification of drugs of abuse is still a challenge, once the access to drug standards is very restricted in Brazil. In this work, ecstasy tablets seized by the Brazilian Federal Police have their chemical composition identified and quantified by gas chromatography and quantitative 1 H nuclear magnetic resonance based on an internal standard approach (IS-1 H-qNMR). Both methods were validated and showed suitable results for the figures of merit. IS-1 H-qNMR shows excellent results of accuracy (relative error < 5%) and precision (relative standard deviation (RSD) < 2%). Comparatively, IS-1 H-qNMR is more efficient and versatile than gas chromatography to accomplish in a single analysis the identification and quantification of target analytes. Since the method does not require a specific reference material, it is cost effective and provides agility to routine forensic analysis.

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

“…In this study, quantitative analysis of different selected samples of MDMA/NPS powder and crystal mixtures was achieved, with simple extraction using D 2 O containing MA (2.0 mg mL À1 ) as an IS (Table 1). 16,20 Initially the samples were identied and characterized using 1D/2D NMR and LC-ESI/MS. Structural elucidation allowed the selection of signals for quantication of each component with high condence.…”

“…This has been deemed sufficient with 100% recovery according to the literature. 20,28 Additionally, numerous tablets were qualitatively analysed for cutting agents and types of excipients using NMR. The UHPLC method gave a good linearity on plotting the concentration (mg mL À1 ) against UV response (Fig.…”

“…16 Similarly, in independent studies, Maldaner, de Oliveira and co-workers quantied MDMA by GC-FID and 1 H q-NMR (at 600 MHz) also using MA as the IS. 20 NMR was shown to be more efficient and versatile than GC in accomplishing the identication and quantication of target analytes in a single analysis with excellent results of accuracy (relative error < 5%) and precision (relative standard deviation, RSD < 2%). Another strength of the NMR method is that it does not require a specic reference material for analysis.…”

“…The MDMA$HCl purity ranged from 10 to 77%, a mass of 39-152 mg per tablet. 20 Recent research has led to the rapid identication of NPS, including MDMA, using a low-eld (LF) (60 MHz) benchtop 1 H NMR spectrometer. 21 Indeed, the screening, detection and quantication of illicit drug "spice" samples using LF NMR spectroscopy has been explored by Gilard and co-workers showing that the recent introduction of benchtop cryogen-free LF NMR spectrometers (60 MHz) can provide useful insights, in the form of diagnostic signals, to chemical structure.…”

Preparation of terpolymer capsules containingRosmarinus officinalisessential oil and evaluation of its antifungal activity

“…To obtain the spectra was used the NMR equipment Bucker 600 Ascend, installed at the Central Analítica of the Institute of Chemistry of the University of Brasília, equipped with a 5 mm probe operating at 600 MHz. About 10 mg of the sample and 10 mg of the internal standard benzoic acid were dissolved in 1 mL of chloroform deuterated and the spectra were acquired at 25 C. 18…”