Ecstasy Tablets Research Articles

Identification of MDA in seized ecstasy-like samples using atmospheric solids analysis probe mass spectrometry and machine learning

In this study, a total of 64 samples of ecstasy tablets seized during operations conducted within the State of Rio Grande do Sul – Brazil in 2021–2022 were analyzed. The instrumental analysis was performed using the Radian ASAP MS instrument with a single quadrupole mass spectrometer and an Atmospheric Solids Analysis Probe (ASAP) interface. Data preprocessing was conducted using MATLAB to improve data quality for subsequent chemometric analyses. Classification models seeking to identify samples containing MDA (3,4-methylenedioxyamphetamine) were developed using Linear Discriminant Analysis (LDA) with variable selection through the genetic algorithm (GA), stepwise (SW), and successive projections algorithm (SPA). Additionally, Partial Least Squares Discriminant Analysis (PLS-DA) models were explored. The GA-LDA model achieved an accuracy of approximately 95% for both training and testing sets, demonstrating its effectiveness in distinguishing between sample classes. It selected only five variables during model building. The SW-LDA model displayed exceptional performance in the training set, achieving 100% for all metrics. However, its accuracy for the testing set was slightly lower at 84.7%, suggesting potential overfitting due to the inclusion of numerous variables. The SPA-LDA model, while not the best performer in the testing set, selected variables that were more easily attributed to specific ions/fragments, aiding in the interpretation of results. Interpretation of selected variables revealed key m/z values associated with different compounds found in the samples, such as MDMA, cocaine, and amphetamine-related fragments. Notably, the SPA method selected six variables that played a crucial role in distinguishing between sample groups. These findings contribute to the advancement of forensic drug analysis and quality control processes.

Chemical composition of Ecstasy tablets seized in Poland between 2005 and 2020.

The most commonly associated substance found in Ecstasy tablets is MDMA (3,4-methylenedioxymethamphetamine). In our study, we showed how the composition of psychoactive ingredients in Ecstasy tablets seized on the drug market in Poland has changed in the years 2005-2020. The study material consisted of nearly 20,000 single Ecstasy tablets seized by representatives of law enforcement (the police, prosecutors) from 2005 to 2020 and analysed by the Institute of Forensic Research, Krakow, Poland. The analysis of the tablets was carried out by gas chromatography-mass spectrometry (GC-MS), high-performance liquid chromatography with diode array detection (HPLC-DAD) and ultra-high-performance liquid chromatography with photodiode array detection (UHPLC-PDA). Currently, new types of MDMA tablets are introduced onto the market, available in various colours and shapes. Our study showed that tablets sold on the street as Ecstasy have variable purity and sometimes contain little or no MDMA. The mean content of MDMA in one tablet seized in 2005-2011 decreased from 90 to 50mg. In 2013, Ecstasy tablets with a very high MDMA content (average 195mg per tablet) appeared on the market, but in the next 2years, the MDMA content decreased again. From 2016, the average MDMA content began to rise again, ranging from 60 to 280mg. Tablets sold as Ecstasy also contained completely different psychoactive substances, including new psychoactive substances (NPS) (found in almost 20% of all examined tablets sold as Ecstasy) belonging to different chemical groups or their dangerous combinations (i.e. phenylethylamines, piperazines, tryptamines, cathinones, arylalkylamines, arylcyclohexylamines and piperidines). Such a large variety of psychoactive substances in Ecstasy tablets is associated with a high risk for users unaware of their composition.

Performance assessment of portable Raman spectroscopy in determining ecstasy tablets

AbstractEcstasy tablets, a type of common street drug originally consisting of 3,4‐methylenedioxymethamphetamine (MDMA), provide stimulant and hallucinogen psychoactive effects. They are frequently found in nightclubs, musical festivals or other recreational events believed to create a relaxing experience for the users. From a forensic perspective, when the drug of abuse is suspected in such scenarios, the law enforcement personnel would then require an easy‐to‐perform, quick and accurate method to detect the existence of such controlled substance prior to the seizure and subsequent forensic examination. In this study, we assessed the performance of a portable Raman spectroscopy as the primary aid in determining ecstasy tablets at the point of use. A total of 130 ecstasy tablet samples were analysed by Raman spectroscopy and characterised by gas chromatography–mass spectrometry (GC–MS). Active chemical substances and cutting agents detected by the two instrumentations were then compared. The performance of Raman spectroscopy was further assessed in terms of its accuracy, sensitivity and specificity, corresponding to the analysis results obtained from GC–MS analysis. Overall, portable Raman Spectroscopy used in this study shows an accuracy of 85.4% in analysing ecstasy tablets obtained from case samples, while the sensitivity and specificity were determined as 85.2% and 100%, respectively. No false positives for MDMA or other drugs were reported. Our results show that portable Raman spectroscopy is a suitable technique for targeted determination of the presence of ecstasy tablets, especially in forensic cases that require non‐destructive, rapid and mass screening during on‐site testing by law enforcement personnel.

Qualitative transformations of street-seized ecstasy over a decade: A case study in Rio de Janeiro (Brazil).

The illegal drug market is constantly evolving, with new drugs being created and existing ones being modified. Adulterants are often added to the mix, and the primary substance may be secretly replaced by a new one. Once-known tablets can now be vastly different from what they are sold as, all due to the pursuit of profit and evasion of current drug regulations. These alterations in drug composition pose a threat to society, as their effects are still not well understood. Therefore, it is crucial for police intelligence and public health development to obtain the chemical profiles of illicit drugs. This study presents the chemical fingerprinting of ecstasy tablets seized in the state of Rio de Janeiro (Brazil) between 2012 and 2021. The tablet samples were weighed, extracted, diluted with methanol, and acidified before analysis using gas chromatography high-resolution mass spectrometry and attenuated total reflection Fourier transform infrared spectroscopy. The major constituents found were MDMA and clobenzorex, with fewer occurrences of MDA, MDEA, and 2C-B. The results also indicate that the occurrence of mega-events in the study location impacted the chemical fingerprints of ecstasy. A total of 27 combinations of cutting agents, including caffeine, ephedrine, and anesthetics, were identified. Samples composed of clobenzorex were observed throughout the evaluated period in areas near highways, suggesting that this product is mainly used by truck drivers. These findings can help police intelligence units anticipate the behavior of the illicit market during major events, identify traffic routes, and support public health initiatives.

Przestępstwo zmowy (conspiracy) w amerykańskim prawie karnym a przestępstwo udziału w zorganizowanej grupie przestępczej lub związku przestępczym

The article is based on the opinion of an expert in American criminal law drawn up in the course of proceedings before a Polish district court. In these proceedings, one of the defendants was charged, among other things, with participation in an organized criminal group whose purpose was to export from Poland without the required regulatory authorization and to illegally trade after importing into the United States of America a psychotropic substance in significant quantities in the form of ecstasy tablets containing the substance MDMA, i.e. an act under Article 258 § 1 of the Criminal Code. At the same time, in the course of the proceedings, information was obtained that the defendant had already been convicted in the territory of the United States of America for a crime described as “conspiracy to distribute and possession of MDMA for the purpose of distribution”, i.e. an act criminalized by Article 21 the United States Code § 846. In connection with the above, it became necessary in the proceedings to determine whether there was an identity in subject matter between the crime charged against the defendant in the proceedings before the Polish court and the crime for which he had been convicted in the territory of the United States. The purpose of the article is to analyze whether the crime of participation in an organized criminal group described in Polish law in Article 258 § 1 of the Criminal Code can be understood as the crime of conspiracy to commit a crime criminalized in American federal law under 21 U.S.C. § 846.

Oxygen plasma-treated graphite sheet electrodes: A sensitive and disposable sensor for methamphetamines

3,4-methylenedioxymethamphetamine (MDMA) is a drug of abuse, known as ecstasy, and it is among the most consumed drugs worldwide. The presence of MDMA and new psychoactive substances has been widely reported in seized forensic samples. The development of an elective and sensitive screening method for MDMA detection is very important in the current scenario of illicit drugs. In this paper, we present affordable graphite sheet (GS) electrodes a new sensing platform for MDMA detection. Importantly, a surface treatment protocol for these electrodes using cold plasma improves the electrochemical response of MDMA. The XPS results showed that O2 plasma treatment changed the GS electrode surface, creating oxide groups. GSs were characterized before and after treatment by scanning electron microscopy and electrochemical impedance spectroscopy, and the results suggested a higher surface area and lower resistance to the charge transfer for treated GS electrodes. Using differential pulse voltammetry, it was possible to achieve a linear range from 0.5 to 15.0 µmol L−1 with a low limit of detection (0.09 µmol L−1). Higher interaction of MDMA with the plasma-treated GS surface (in comparison with the pristine surface) was confirmed by computational simulations (molecular dynamics), which may explain the improved sensing properties provided by the plasma treatment. Additionally, the interference study with other drugs usually found in seized ecstasy tablets showed high selectivity which enabled MDMA detection in human saliva (collected in parties and electronic music festivals) and seized samples. Therefore, plasma-treated GS can be used as a simple, fast, low-cost, and portable screening device for application in real-world forensic samples.

Using ATR-FTIR spectroscopy and DD-SIMCA for ecstasy profiling

Ecstasy is a recreational drug known to have serious adverse effects, necessitating the development of new techniques for its rapid and affordable identification in harm reduction policies and forensic laboratories. In this study, ATR-FTIR spectroscopy and DD-SIMCA (Data Driven Soft Independent Modeling of Class Analogy) were employed to determine the profile of ecstasy tablets and their adulterants. ATR-FTIR spectroscopy, which is a fast and non-destructive method that provides structural information, and DD-SIMCA, a supervised technique that distinguishes between different groups, were used. The Hierarchical Cluster Analysis (HCA) revealed the formation of two primary clusters: one comprising mainly MDA samples with some MDMA samples, and the second including cocaine, methamphetamine, and caffeine samples, as well as a mixture of MDA samples with methamphetamine and caffeine. Principal Component Analysis (PCA) was performed, and the first five principal components (PC) explained 86.25% of the total data variance. In the PC1xPC2 scores plot, the distribution of samples containing MDs (MDA and MDMA) was observed. Further analysis using PCA revealed the grouping of cocaine samples into two separate groups based on variations in concentration. The DD-SIMCA model demonstrated high sensitivity values in accurately identifying target samples (MDA) and relatively high specificity values in both the training and test sets. The study highlights the effectiveness of ATR-FTIR spectroscopy, PCA, and DD-SIMCA for the precise classification of ecstasy and its adulterants and suggests their potential in drug identification and analysis.

An overview of New Psychoactive Substances (NPS) in northeast Brazil: NMR-based identification and analysis of ecstasy tablets by GC-MS

The actual illicit market for synthetic drugs is characterized by a wide variety of psychoactive substances of different chemical and pharmacological classes, such as amphetamine-type stimulants and new psychoactive substances. The knowledge about its chemical composition, as well as the nature and quantity of the active substances present, is important for emergency care in intoxication cases by these substances and to establish adequate chemical and toxicological analysis procedures in forensic laboratories. The aim of this work was to study the prevalence of amphetamine-type stimulants and new psychoactive substances in the states of Bahia and Sergipe, in the northeast region of Brazil, involving samples of drugs seized by the local police forces from 2014 to 2019. In a total of 121 seized and analyzed samples, in which ecstasy tablets predominated (n = 101), nineteen substances were identified using GC-MS and 1D NMR techniques, comprising classical synthetic drugs and new psychoactive substances (NPS). In order to determine the composition of ecstasy tablets, an analytical method based on GC-MS was applied after validation. Analyzes of 101 ecstasy tablets showed that MDMA was the main substance, being found in 57% of the samples, in amounts between 27.3 and 187.1 mg per tablet. In addition, mixtures of MDMA, MDA, synthetic cathinones and caffeine were observed in 34 samples. These results demonstrate that the variety of substances found and the composition of seized materials in northeast Brazil is similar to other studies carried out previously in other Brazilian regions.

Uticaj pandemije COVID-19 na nasilni ekstremizam i organizovani kriminal u Republici Srbiji

The subject of research is the impact of the COVID-19 pandemic on violent extremism and organized crime in the Republic of Serbia. The authors used the method of document content analysis and quantitative methods (surveys) for research purposes. The time of the research included the most intense period of the pandemic, and the authors investigated the situation in the Republic of Serbia from March 2020, when the virus was first registered, to mid-2021. The initial hypothesis in the research is that violent extremism and organized crime adapt very quickly to new social changes, which makes them resilient to many social crises. Serbia has a long history of fighting etno-separatist extremism (e.g. the KLA terrorist organization), but the COVID-19 pandemic has intensified the growth of other forms of extremism, such as religious, left-wing, while special attention is focused on right-wing extremism. Namely, the authors determined that in addition to the old generators (what is the post-conflict legacy), we also have two new crucial generators of the extreme right - the COVID-19 pandemic and the migrant crisis. All the fundamental issues on which the extreme right-wingers built their ideology (such as Kosovo and Metohija, the friend-enemy dichotomy) were pushed aside during the pandemic, in order to actualize the problems concerning the "infestation of migrants", conspiracy theories, vaccinations, 5G networks and of panic fear for the survival of the nation. Organized crime also found a way to adapt to the pandemic, and some new areas appeared that criminals quickly prioritized, such as the trade-in of deficient medical equipment, falsification of PCR tests, etc. Drug trafficking was particularly intense, and the Customs Administration seized during the pandemic from 01.03.2020 to 01.08.2021 5630.53 grams of cocaine, which is 60 percent more than in 2019; 2063 grams of heroin, which is a drop to only 5 percent of the total seizure in 2019. In the same period, 1,180 tablets of ecstasy and MDMA were seized, which is five times more than in 2019, as well as 36 weapons. The conclusion is that the COVID-19 pandemic had a significant impact on the change in the functioning of violent extremism and organized crime, thus confirming the initial hypothesis of the author, that these are "tough phenomena" that adapt very quickly and easily to emerging social crises. which is down to just 5 percent of total seizures in 2019. In the same period, 1,180 tablets of ecstasy and MDMA were seized, which is five times more than in 2019, as well as 36 weapons. The conclusion is that the COVID-19 pandemic had a significant impact on the change in the functioning of violent extremism and organized crime, thus confirming the initial hypothesis of the author, that these are "tough phenomena" that adapt very quickly and easily to emerging social crises. which is down to just 5 percent of total seizures in 2019. In the same period, 1,180 tablets of ecstasy and MDMA were seized, which is five times more than in 2019, as well as 36 weapons. The conclusion is that the COVID-19 pandemic had a significant impact on the change in the functioning of violent extremism and organized crime, thus confirming the initial hypothesis of the author, that these are "tough phenomena" that adapt very quickly and easily to emerging social crises.

Different types of pharmaceutical tablets used for treatment of diseases

In modern age of revolution and development in drug delivery for better clinical effects conventional dosages form have still a strong grip and most popular in all kinds of medicinal preparation intended for oral use. To satisfy the need of growing market tablets dosages form have incorporated modernization in producing and some advanced tablet types. Modified release tablet formulations including, layered tablets such as In +--lay tablet, Bi-layered tablet, Medicated chewing gum, Tablet tarts, Pastilles, Lollipop, Tablet inserts, Clinicaps, Caplets, Child ecstasy tablet and Tablet in tablet are new entries in pharmaceutical market. This review highlights the current advancements and patents in tablet technology. Recent advances in novel drug delivery system (NDDS) aims to enhance safety and efficacy of drug molecule by formulating a convenient dosage form for ease of administration and to achieve better patient compliance. In the recent trend one such approach the development of rapid disintegrating tablets formulation is emerging and gaining popularity because it is easy to administer and leads to better patient compliance. These dosage forms are placed in the mouth, allowed to disperse or dissolve in the saliva. They release the drug as soon as they come in contact with the saliva, thus obviating the need for water during administration. The aim of this article is to review the progress of the evolving technologies and super disintegrating agents in the formulation, manufacturing and evaluation of these tablets. This article also discusses the new evaluation methodologies for these rapid disintegrating tablets. Various modifications in the conventional evaluation and use of specialized instruments are found to be essential in the testing of these dosage forms. In the present review the formulation techniques and different technologies are discussed.

Size matters: comparing the MDMA content and weight of ecstasy tablets submitted to European drug checking services in 2012–2021

Purpose The 3,4-methylenedioxymetamphetamine (MDMA) content in ecstasy tablets has increased enormously throughout Europe across the past decade. This study aims to determine whether this is caused by the production of “stronger” tablets (more mg MDMA per mg of tablet), or if tablets have simply been getting larger and heavier (more mg of tablet in total). Design/methodology/approach A data set of 31,716 ecstasy tablets obtained in 2012–2021 by 10 members of the Trans European Drug Information (TEDI) network was analysed. Findings The MDMA mass fraction in ecstasy tablets has remained virtually unchanged over the past 10 years, with increased MDMA contents being attributed almost exclusively to increased tablet weight. These trends seem to be uniform across Europe, despite varying sampling and analytical techniques being used by the TEDI participants. The study also shows that while tablet weight correlates perfectly with MDMA content on a yearly basis, wide variations in the MDMA mass fraction make such relations irrelevant for determining the MDMA content of individual tablets. Research limitations/implications These results provide new opportunities for harm reduction, given that size is a tangible and apparently accurate characteristic to emphasise that one tablet does not simply equate to one dose. This is particularly useful for harm reduction services without the resources for in-house quantification of large numbers of ecstasy tablets, although the results of this study also show that chemical analysis remains crucial for accurate personalised harm reduction. Originality/value The findings are both new and pertinent, providing a novel insight into the market dynamics of ecstasy tablet production at a transnational level.

On-site forensic analysis of colored seized materials: Detection of brown heroin and MDMA-tablets by a portable NIR spectrometer.

The increasing workload for forensic laboratories and the expanding complexity of the drug market necessitates efficient approaches to detect drugs of abuse. Identification directly at the scene of crime enables investigative forces to make rapid decisions. Additionally, on-site identification of the material also leads to considerable efficiency and cost benefits. As such, paperwork, transportation, and time-consuming analysis in a laboratory may be avoided. Near-infrared (NIR) spectroscopy is an analysis technique suitable for rapid drug testing using portable equipment. A possible limitation of spectroscopic analysis concerns the complexity of seized materials. NIR measurements represent composite spectra for mixtures and diagnostic spectral features can be obscured by excipients such as colorants. Herein, a NIR-based (1300-2600 nm) detection of heroin and MDMA in colored casework (i.e., brown powders and ecstasy tablets) using a portable analyzer is presented. The application includes a multistage data analysis model based on the net analyte signal (NAS) approach. This identification model was specifically designed for mixture analysis and requires a limited set of pure reference spectra only. Consequently, model calibration efforts are reduced to a minimum. A total of 549 forensic samples was tested comprising brown heroine samples and a variety of colored tablets with different active ingredients. This investigation led to a >99% true negative and >93% true positive rate for heroin and MDMA. These results show that accurate on-site detection in colored casework is possible using NIR spectroscopy combined with an efficient data analysis model. These findings may eventually help in the transition of routine forensic laboratories from laboratory-based techniques to portable equipment operated on scene.

Portable Raman spectroscopy applied to the study of drugs of abuse.

The use of drugs of abuse has grown significantly in recent decades. In forensic chemistry, methods of identifying and characterizing illicit drugs contribute to the interests of researchers, experts, and public security authorities. Among existing methods, portable Raman spectroscopy is notable for performing rapid, non-destructive, and highly selective analysis in the laboratory or on-site. When the resulting spectral data are paired with chemometric tools, methods of exploratory analysis and multivariate calibration can be developed. Thus, this work describes the application of Raman spectroscopy associated with principal component analysis (PCA) and interval principal component analysis (iPCA) to assessing trends in samples of cocaine (n= 40), crack (n= 33), and their main adulterants (n= 5) and diluents (n= 5), tablets of ecstasy (n= 14), designer drugs papers (n= 27), and alcoholic solutions adulterated with benzodiazepines (alprazolam and diazepam). In addition, competitive adaptive reweighted sampling (CARS) combined with partial least squares (PLS) regression (CARSPLS) was used to quantify adulterants (benzocaine, lidocaine, and procaine) in binary mixtures with crack (n= 21) and solutions of cachaça adulterated with bromazepam (n= 11).

On-site illicit-drug detection with an integrated near-infrared spectral sensor: A proof of concept

Illicit-drug production, trafficking and seizures are on an all-time high. This consequently raises pressure on investigative authorities to provide rapid forensic results to assist law enforcement and legal processes in drug-related cases. Ideally, every police officer is equipped with a detector to reliably perform drug testing directly at the incident scene. Such a detector should preferably be small, portable, inexpensive and shock-resistant but should also provide sufficient selectivity to prevent erroneous identifications. This study explores the concept of on-site drugs-of-abuse detection using a 1.8 × 2.2 mm2 multipixel near-infrared (NIR) spectral sensor that potentially can be integrated into a smartphone. This integrated sensor, based on an InGaAs-on-silicon technology, exploits an array of resonant-cavity enhanced photodetectors without any moving parts. A 100% correct classification of 11 common illicit drugs, pharmaceuticals and adulterants was achieved by chemometric modelling of the response of 15 wavelength-specific pixels. The performance on actual forensic casework was investigated on 246 cocaine-suspected powders and 39 MDMA-suspected ecstasy tablets yielding an over 90% correct classification in both cases. These findings show that presumptive drug testing by miniaturized spectral sensors is a promising development ultimately paving the way for a fully integrated drug-sensor in mobile communication devices used by law enforcement.

3,4-Methylenedioxymethamphetamine quantification via benchtop 1H qNMR spectroscopy: Method validation and its application to ecstasy tablets collected at music festivals

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.

The Cathinone Hydra: Increased Cathinone and caffeine adulteration in the English MDMA market after Brexit and COVID-19 lockdowns

Adulteration poses additional unknown risks to the health of people who use illicit drugs. In this study, we sought to determine the extent and nature of adulteration of ‘MDMA’ in circulation at English summer music festivals in 2021, following Brexit, COVID-19 lockdowns and various regulatory changes overseas. At three festivals in 2019 and 2021, 1648 surrendered substances were analysed with Fourier-transform infrared spectroscopy and colourimetric reagents in a mobile laboratory as part of a harm reduction project. Form, mass, appearance and main psychoactive component were recorded. Analytical results were compared to a parallel self-report survey with 1124 attendees at the same events, as part of the annual English Festival Study. In 2019 and 2021, 417 and 377 samples strongly resembling MDMA (e.g. ecstasy tablets) were tested. Detection of MDMA in such samples decreased from 93% to 55% between the two years. Whilst virtually absent in 2019, synthetic cathinones and caffeine each constituted approximately one fifth of 2021 samples. 4-Chloromethcathinone (4-CMC), 3-methylmethcathinone (3-MMC) and N-ethylbutylone (eutylone) were the most prevalent cathinones detected. In both years, >35% of survey respondents reported use and/or intention to use MDMA on the fieldwork day; ≤1% reported cathinone or caffeine use, suggesting their consumption was predominantly unintentional. The sharp rise in synthetic cathinone prevalence in the summer 2021 UK market coincided with a unique combination of events including Brexit and the reopening of nightlife after 16 months of lockdowns, months ahead of other European nations. Echoing similar periods over the past decade, the cathinone hydra reared its head to satisfy the buoyant demand for MDMA at a time of scarcity, through substitution with substances legally obtainable in the Netherlands at the time of data collection. Alerts issued on social media led to >360,000 engagements, demonstrating extensive public engagement with illicit market monitoring and harm reduction advice.

Fast on-site screening of 3,4-methylenedioxyethylamphetamine (MDEA) in forensic samples using carbon screen-printed electrode and square wave voltammetry

The worldwide seizures of illicit synthetic drugs have been dramatically increasing over the past decade, when the quantity of seized amphetamine-type stimulants (ATS) quadrupled, while seized ecstasy (3,4–methylenedioxymethamphetamine or MDMA)-like substances doubled. In this work, a simple and fast methodology for the electrochemical screening of ecstasy analogue MDEA (3,4-methylenedioxyethylamphetamine) in forensic samples is presented, for the first time, using a carbon screen-printed electrode (C-SPE) and square wave voltammetry (SWV). The electrochemical behavior of MDEA was studied by cyclic voltammetry at different pH values (2 to 12), where an altered electrochemistry of this drug on C-SPE, with an unreported redox pair, was observed in comparison with previous works dealing with the voltammetric detection of other ATS with similar chemical structures. Based on the acquired electrochemical processes, a redox reaction mechanism for MDEA on C-SPE is proposed. The best conditions (sensitivity and selectivity) for MDEA screening were obtained by SWV (a: 40 mV, f: 30 Hz, and Estep: 4 mV) and 0.04 mol L−1 Britton Robinson buffer solution at pH 3.0 as the supporting electrolyte. The proposed method presents a wide linear range (2.5 to 30.0 µmol L−1, R2 > 0.99), high sensitivity (0.569 µA / µmol L−1), low theoretical limit of detection (0.03 µmol L−1), and good repeatability using the same C-SPE (RSD < 6%; n = 10). The inter-device reproducibility (n = 5) showed a minimal variation of peak potentials (RSD < 2.3%). The interference study was performed with some adulterants usually found in ecstasy tablets, such as paracetamol, caffeine, glucose, ketamine, cocaine, acetylsalicylic acid, amphetamine (A), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), MDMA, ethylone (bk-MDEA), n-ethylpentylone (bk-EBDP) and dibutylone (bk-DMDBD). The method was applied in real seized samples containing MDEA with addition-recovery studies close to 100%. The developed method is promising to be used as a preliminary test for the screening of MDEA in the ever-changing situation concerning seized forensic samples. The proposed sensor exhibits attractive features for application in forensic analysis, such as rapidness, simplicity, low-cost, user friendly and portability.

Electrochemical detection of MDMA and 2C-B in ecstasy tablets using a selectivity enhancement strategy by in-situ derivatization

Forensic drug laboratories are confronted with increasing amounts of drugs and a demand for faster results that are directly available on-site. In addition, the drug market is getting more complex with hundreds of new psychoactive substances (NPS) entering the market in recent years. Rapid and on-scene presumptive drug testing therefore faces a shift from manual colorimetric tests towards approaches that can detect a wider range of components and process results automatically. Electrochemical detection offers these desired characteristics, making it a suitable candidate for on-site drug detection. In this study, a two-step electrochemical sensor is introduced for the detection of MDMA and 2C-B. Firstly, a direct electrochemical analysis was performed to detect MDMA. Validation experiments on over 70 substances revealed that 2C-B was the only frequently encountered drug that gave a false positive result for MDMA in this first analysis. A second step using in-situ derivatization was subsequently introduced. To this end, formaldehyde was used for N-methylation of 2C-B thereby enhancing its electrochemical profile. The enriched electrochemical fingerprint in the second step allowed for clear differentiation between MDMA and 2C-B. The applicability of this approach was demonstrated with 71 ecstasy tablets seized by the Amsterdam Police. The MDMA/2C-B sensor correctly identified all 39 MDMA-containing tablets and 10 out of 11 tablets containing 2C-B. Most notably, correct results were also obtained for dark colored tablets in which both spectroscopic analysis and colorimetric tests failed due to obscured signals.

Ecstasy tablets: Rapid identification and determination of enantiomeric excess of MDMA

The consumption of psychoactive substances is a worldwide problem and the sheer number of their seizures is alarming. These substances also include the synthetic drug 3,4-methylenedioxy-N-methylamphetamine (MDMA), also known as ecstasy, which is very often abused and widespread around the world. The number of ecstasy tablet seizures testifies to their popularity, especially on the dance music scene. One chiral center can be found in the MDMA molecule and therefore it may occur as two enantiomers, which are characterized by different physiological activity. Therefore, knowledge of the enantiomeric excess in the seized tablets is highly desirable. Within the work, dimensional and weight analysis were performed supported by photographic documentation. In addition, Raman and infrared (IR) spectroscopy were used to verify the content of the active substance in the tablets. Subsequently, the electronic circular dichroism (ECD) was used to construct a calibration curve for the determination of the enantiomeric excess of MDMA in the seized tablets. The obtained results show that most of the seized tablets contained MDMA as a racemate.

Paper spray ionization coupled to Fourier Transform Ion Cyclotron Resonance Mass Spectrometry as a tool to fight the counterfeiting of medicines

Analyses of illicit drugs and medicines in forensic laboratories require constant improvements and updates in protocols and analytical techniques in order to follow the new trends employed by illicit producers. Therefore, applying reliable and fast techniques to perform the chemical profiling of seized samples, allowing for detection of the different types of falsification performed, is an urgent measure. In this study, Paper Spray Ionization (PSI) coupled to Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS) was used for determining the chemical profiling of 92 samples of counterfeit medicines and ecstasy tablets. Afterwards, all the samples were evaluated using principal component analysis (PCA) to distinguish their chemical composition. From the results, different strategies for medicine counterfeiting were identified, such as changing the API and employing a mixture of substances to produce distinct medicines. Cross contamination of medicines with cocaine and 3,4-methylenedioxymethamphetamine (MDMA) was also detected. Moreover, the compounds cassaidine and glyceryl nonivamide were identified in all three classes of the seized medicines analyzed. Such compounds act as new markers in illicit production, not reported before in counterfeit medicines. The majority of ecstasy tablets contained MDMA and ethylone in their composition. Using PSI-MS combined with chemometrics, substances present in the seized medicines and ecstasy tablets could be detected through a simple, fast, and reliable procedure. Therefore, it was possible to connect the substances present in the seized material according to their chemical profiling, thus producing important evidence for police intelligence, which constitutes a great tool to be employed in forensic laboratories.