TY - JOUR
T1 - 3,4-Methylenedioxymethamphetamine Quantification via Benchtop 1H qNMR Spectroscopy: Method Validation and its Application to Ecstasy Tablets Collected at Music Festivals
AU - Frinculescu, Anca
AU - Maier, Alexander
AU - Shine, Trevor
AU - Ramsey, John
AU - Araneda, Juan
AU - Riegel, Susanne
AU - Frascione, Nunzianda
AU - Abbate, Vincenzo
N1 - Funding Information:
The authors would like to acknowledge Orapan Apirakkan and Giuseppe Floresta from King's College London, Dee Gill from GPE Scientific, and Maria del Mar Boronat Ena for their support.
Publisher Copyright:
© 2022 Elsevier B.V.
PY - 2022/5/30
Y1 - 2022/5/30
N2 - We describe a method validation for the quantification of 3,4-methylenedioxymethamphetamine (MDMA) in tablets based on the United Nations Office on Drugs and Crime (UNODC) guideline for quantitative Nuclear Magnetic Resonance analysis (qNMR). qNMR experiments were carried out on a 60 MHz benchtop NMR spectrometer employing ethylene carbonate as an internal calibrant. A series of ‘ecstasy’ tablets seized at music events were quantified and the results discussed regarding their within-batch variation and yearly median dose. The method showed good specificity and selectivity, with linearity, precision, accuracy, and recovery well within the UNODC recommended criteria. The limit of detection and quantification are 0.33 mg/mL and 0.10 mg/mL respectively, proving the method works well on small amounts of MDMA. Overall, the lowest amount of MDMA free base detected in this study was 9.35 mg in a piperazine mix, while the highest dosed tablet contained 237.55 mg MDMA free base, with a 9.1% decrease in median amount compared to the pre-pandemic data (2019), but still higher than the data collected in a previous study (105 mg median amount of MDMA free base in 2018). The within-batch variation was insignificant for one of the seizures but showed greater variation for the other, which confirmed that the MDMA content of a single tablet may not reflect that of the whole batch. This dynamic upward change in tablet dosage highlights the importance of ongoing trend monitoring and specific prevention intervention to counteract the negative consequences associated with MDMA use. Benchtop NMR has been successfully employed in quality control, material science and more recently, drug analysis. The present study demonstrates its beneficial application in forensic science overcoming the limitations of currently available instruments and techniques employed in harm reduction and field testing.
AB - We describe a method validation for the quantification of 3,4-methylenedioxymethamphetamine (MDMA) in tablets based on the United Nations Office on Drugs and Crime (UNODC) guideline for quantitative Nuclear Magnetic Resonance analysis (qNMR). qNMR experiments were carried out on a 60 MHz benchtop NMR spectrometer employing ethylene carbonate as an internal calibrant. A series of ‘ecstasy’ tablets seized at music events were quantified and the results discussed regarding their within-batch variation and yearly median dose. The method showed good specificity and selectivity, with linearity, precision, accuracy, and recovery well within the UNODC recommended criteria. The limit of detection and quantification are 0.33 mg/mL and 0.10 mg/mL respectively, proving the method works well on small amounts of MDMA. Overall, the lowest amount of MDMA free base detected in this study was 9.35 mg in a piperazine mix, while the highest dosed tablet contained 237.55 mg MDMA free base, with a 9.1% decrease in median amount compared to the pre-pandemic data (2019), but still higher than the data collected in a previous study (105 mg median amount of MDMA free base in 2018). The within-batch variation was insignificant for one of the seizures but showed greater variation for the other, which confirmed that the MDMA content of a single tablet may not reflect that of the whole batch. This dynamic upward change in tablet dosage highlights the importance of ongoing trend monitoring and specific prevention intervention to counteract the negative consequences associated with MDMA use. Benchtop NMR has been successfully employed in quality control, material science and more recently, drug analysis. The present study demonstrates its beneficial application in forensic science overcoming the limitations of currently available instruments and techniques employed in harm reduction and field testing.
UR - http://www.scopus.com/inward/record.url?scp=85127033568&partnerID=8YFLogxK
U2 - 10.1016/j.jpba.2022.114728
DO - 10.1016/j.jpba.2022.114728
M3 - Article
SN - 0731-7085
VL - 214
JO - Journal of Pharmaceutical and Biomedical Analysis
JF - Journal of Pharmaceutical and Biomedical Analysis
M1 - 114728
ER -
