PMID- 35349940
OWN - NLM
STAT- MEDLINE
DCOM- 20220426
LR  - 20221014
IS  - 1873-264X (Electronic)
IS  - 0731-7085 (Linking)
VI  - 214
DP  - 2022 May 30
TI  - 3,4-Methylenedioxymethamphetamine quantification via benchtop (1)H qNMR 
      spectroscopy: Method validation and its application to ecstasy tablets collected 
      at music festivals.
PG  - 114728
LID - S0731-7085(22)00149-2 [pii]
LID - 10.1016/j.jpba.2022.114728 [doi]
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.
CI  - Copyright (c) 2022 Elsevier B.V. All rights reserved.
FAU - Frinculescu, Anca
AU  - Frinculescu A
AD  - Department of Analytical, Environmental and Forensic Sciences, King's College 
      London, 150 Stamford Street, London SE1 9NH, United Kingdom; TICTAC 
      Communications Ltd., Room 1.159 Jenner Wing, St. George's University of London, 
      Cranmer Terrace, London SW17 0RE, United Kingdom.
FAU - Maier, Alexander F G
AU  - Maier AFG
AD  - Nanalysis Corp., 1, 4600 5 Street NE, Calgary, AB T2E 7C3, Canada.
FAU - Shine, Trevor
AU  - Shine T
AD  - TICTAC Communications Ltd., Room 1.159 Jenner Wing, St. George's University of 
      London, Cranmer Terrace, London SW17 0RE, United Kingdom.
FAU - Ramsey, John
AU  - Ramsey J
AD  - TICTAC Communications Ltd., Room 1.159 Jenner Wing, St. George's University of 
      London, Cranmer Terrace, London SW17 0RE, United Kingdom.
FAU - Araneda, Juan F
AU  - Araneda JF
AD  - Nanalysis Corp., 1, 4600 5 Street NE, Calgary, AB T2E 7C3, Canada.
FAU - Riegel, Susanne D
AU  - Riegel SD
AD  - Nanalysis Corp., 1, 4600 5 Street NE, Calgary, AB T2E 7C3, Canada.
FAU - Frascione, Nunzianda
AU  - Frascione N
AD  - Department of Analytical, Environmental and Forensic Sciences, King's College 
      London, 150 Stamford Street, London SE1 9NH, United Kingdom.
FAU - Abbate, Vincenzo
AU  - Abbate V
AD  - Department of Analytical, Environmental and Forensic Sciences, King's College 
      London, 150 Stamford Street, London SE1 9NH, United Kingdom. Electronic address: 
      vincenzo.abbate@kcl.ac.uk.
LA  - eng
PT  - Journal Article
DEP - 20220316
PL  - England
TA  - J Pharm Biomed Anal
JT  - Journal of pharmaceutical and biomedical analysis
JID - 8309336
RN  - 0 (Hallucinogens)
RN  - 0 (Illicit Drugs)
RN  - 0 (Tablets)
RN  - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine)
SB  - IM
CIN - J Pharm Biomed Anal. 2022 Nov 30;221:115042. PMID: 36155482
MH  - *Hallucinogens/analysis
MH  - Holidays
MH  - *Illicit Drugs/analysis
MH  - Magnetic Resonance Spectroscopy
MH  - *Music
MH  - *N-Methyl-3,4-methylenedioxyamphetamine/analysis/chemistry
MH  - Tablets/chemistry
OTO - NOTNLM
OT  - Benchtop NMR
OT  - Illicit drug analysis
OT  - MDMA
OT  - Method validation
OT  - Quantitative analysis
OT  - qNMR
EDAT- 2022/03/30 06:00
MHDA- 2022/04/27 06:00
CRDT- 2022/03/29 20:11
PHST- 2022/01/31 00:00 [received]
PHST- 2022/03/10 00:00 [revised]
PHST- 2022/03/14 00:00 [accepted]
PHST- 2022/03/30 06:00 [pubmed]
PHST- 2022/04/27 06:00 [medline]
PHST- 2022/03/29 20:11 [entrez]
AID - S0731-7085(22)00149-2 [pii]
AID - 10.1016/j.jpba.2022.114728 [doi]
PST - ppublish
SO  - J Pharm Biomed Anal. 2022 May 30;214:114728. doi: 10.1016/j.jpba.2022.114728. 
      Epub 2022 Mar 16.