Screening of 104 New Psychoactive Substances (NPS) and Other Drugs of Abuse in Oral Fluid by LC–MS-MS

2020 ◽  
Vol 44 (7) ◽  
pp. 697-707
Author(s):  
Kelly Francisco da Cunha ◽  
Karina Diniz Oliveira ◽  
Marilyn A Huestis ◽  
Jose Luiz Costa
Keyword(s):  
Oral Fluid ◽  
Drugs Of Abuse ◽  
Matrix Effects ◽  
Synthetic Cannabinoids ◽  
Screening Method ◽  
Simultaneous Detection ◽  
New Psychoactive Substances ◽  
Major Public Health Problem ◽  
Psychoactive Substances ◽  
Wide Range

Abstract New psychoactive substances (NPS) are a major public health problem, primarily due to the increased number of acute poisoning cases. Detection of these substances is a challenge. The aim of this research was to develop and validate a sensitive screening method for 104 drugs of abuse, including synthetic cannabinoids, synthetic cathinones, fentanyl analogues, phenethylamines and other abused psychoactive compounds (i.e., THC, MDMA, LSD and their metabolites) in oral fluid by liquid chromatography–tandem mass spectrometry (LC–MS-MS). The Quantisal™ oral fluid device was used to collect oral fluid samples. The oral fluid–elution buffer mixture (500-μL sample) was extracted with t-butyl methyl ether, and chromatographic separation was performed on a Raptor™ biphenyl column (100 × 2.1 mm ID, 2.7 μm), with a total run time of 13.5 min. Limits of detection were established at three concentrations (0.05, 0.1 or 1 ng/mL) for most analytes, except for acetyl norfentanyl and mescaline (5 ng/mL). Matrix effects were generally <20% and overall extraction recoveries >60%. The highest matrix effect was observed within the synthetic cannabinoid group (PB22, −55.5%). Lower recoveries were observed for 2C-T (47.2%) and JWH-175 (58.7%). Recoveries from the Quantisal™ device were also evaluated for all analytes (56.7–127%), with lower recoveries noted for 25I-NBOMe, valerylfentanyl and mCPP (56.7, 63.0 and 69.9%, respectively). Drug stability in oral fluid was evaluated at 15, 60 and 90 days and at 25, 4 and −20°C. As expected, greater stability was observed when samples were stored at −20°C, but even when frozen, some NPS (e.g., synthetic cannabinoids) showed more than 20% degradation. The method was successfully applied to the analysis of seven authentic oral fluid samples positive for 17 different analytes. The method achieved good sensitivity and simultaneous detection of a wide range of NPS.

scholarly journals Sex and Gender Differences in the Effects of Novel Psychoactive Substances

2020 ◽  
Vol 10 (9) ◽  
pp. 606
Author(s):  
Liana Fattore ◽  
Matteo Marti ◽  
Rafaela Mostallino ◽  
Maria Paola Castelli
Keyword(s):  
Gender Differences ◽  
Illicit Drugs ◽  
Drugs Of Abuse ◽  
Subjective Effects ◽  
Synthetic Cannabinoids ◽  
New Psychoactive Substances ◽  
Sex And Gender ◽  
Psychoactive Substances ◽  
And Gender ◽  
Sex And Gender Differences

Sex and gender deeply affect the subjective effects and pharmaco-toxicological responses to drugs. Men are more likely than women to use almost all types of illicit drugs and to present to emergency departments for serious or fatal intoxications. However, women are just as likely as men to develop substance use disorders, and may be more susceptible to craving and relapse. Clinical and preclinical studies have shown important differences between males and females after administration of “classic” drugs of abuse (e.g., Δ9-tetrahydrocannabinol (THC), morphine, cocaine). This scenario has become enormously complicated in the last decade with the overbearing appearance of the new psychoactive substances (NPS) that have emerged as alternatives to regulated drugs. To date, more than 900 NPS have been identified, and can be catalogued in different pharmacological categories including synthetic cannabinoids, synthetic stimulants (cathinones and amphetamine-like), hallucinogenic phenethylamines, synthetic opioids (fentanyls and non-fentanyls), new benzodiazepines and dissociative anesthetics (i.e., methoxetamine and phencyclidine-derivatives). This work collects the little knowledge reached so far on the effects of NPS in male and female animal and human subjects, highlighting how much sex and gender differences in the effects of NPS has yet to be studied and understood.

scholarly journals New Psychoactive Substances: Evolution in the Exchange of Information and Innovative Legal Responses in the European Union

2020 ◽  
Vol 17 (22) ◽  
pp. 8704
Author(s):  
Maria Rosaria Varì ◽  
Giulio Mannocchi ◽  
Roberta Tittarelli ◽  
Laura Leondina Campanozzi ◽  
Giulio Nittari ◽  
...  
Keyword(s):  
Illicit Drugs ◽  
National Level ◽  
Synthetic Cannabinoids ◽  
Warning System ◽  
Legal Framework ◽  
New Psychoactive Substances ◽  
The European Union ◽  
Psychoactive Substances ◽  
Consumer Safety ◽  
Wide Range

At the end of 2019, the European Monitoring Centre for Drugs and Drug Addiction was monitoring around 790 new psychoactive substances, more than twice the total number of controlled substances under the United Nations Conventions. These substances, which are not subject to international drug controls, include a wide range of molecules, including the assortment of drugs such as synthetic cannabinoids, stimulants, opiates, and benzodiazepines. Most of them are sold as “legal” substitutes for illicit drugs, while others are intended for small groups willing to experiment with them in order to know their possible new effects. At the national level, various measures have been taken to control new substances and many European countries have responded with specific legislation in favor of consumer safety and by extending or adapting existing drug laws to incorporate the new psychoactive substances. Moreover, since 1997, an early warning system has been created in Europe for identifying and responding quickly to the risks of new psychoactive substances. In order to establish a quicker and more effective system to address the criminal activities associated with new dangerous psychoactive substances, the European legal framework has considerably changed over the years.

A Comprehensive HPLC–MS-MS Screening Method for 77 New Psychoactive Substances, 24 Classic Drugs and 18 Related Metabolites in Blood, Urine and Oral Fluid

2020 ◽  
Vol 44 (8) ◽  
pp. 769-783
Author(s):  
Annagiulia Di Trana ◽  
Giulio Mannocchi ◽  
Filippo Pirani ◽  
Nunzia La Maida ◽  
Massimo Gottardi ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Oral Fluid ◽  
Multiple Reaction Monitoring ◽  
Screening Method ◽  
Internal Standard ◽  
New Psychoactive Substances ◽  
Spectrometric Analysis ◽  
Blood Proteins ◽  
Psychoactive Substances ◽  
Better Than

Abstract To date, more than 800 molecules are classified as New Psychoactive Substances (NPS), and it is reported that this number increases every year. Whereas several cases of polydrug consumption that led to acute intoxication and death are reported, a lack of effective analytical screening method to detect NPS and classical drug of abuse in human matrices affects the prompt identification of the probable cause of intoxication in emergency department of hospitals. In this concern, a fast, simple and comprehensive high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS-MS) screening method to detect and quantify 77 NPS, 24 classic drugs and 18 related metabolites has been successfully developed and validated in blood, urine and oral fluid. A small volume (100 µL) of whole blood samples spiked with internal standard deuterated mixture was added to 70 µL of M3® buffer, and after precipitation of blood proteins, the supernatant was evaporated to dryness and reconstituted in 1 mL of mobile phase. Same volume (100 µL) of urine and oral fluid samples spiked with internal standard deuterated mix were only diluted with 500 µL of M3® reagent. One microliter of samples of each matrix was injected into HPLC–MS-MS equipment. The run time lasted 10 min with a gradient mobile phase. Mass spectrometric analysis was performed in positive ion multiple reaction monitoring mode. The method was linear for all analytes under investigation with a determination coefficient always better than 0.99. The calibration range for blood and oral fluid was from limits of quantification (LOQs) to 200 ng/mL, whereas that for urine was LOQs to 1000 ng/mL. Recovery and matrix effect were always higher than 80%, whereas intra-assay and inter-assay precision were always better than 19% and accuracy was always within 19% of target in every matrix. Applicability of the method was verified by analysis of samples from real cases.

scholarly journals Development of a New LC-MS/MS Screening Method for Detection of 120 NPS and 43 Drugs in Blood

Separations ◽  
2021 ◽  
Vol 8 (11) ◽  
pp. 221
Author(s):  
Fabio Vaiano ◽  
Elisabetta Bertol ◽  
Maria Mineo ◽  
Laura Pietrosemoli ◽  
Jolanda Rubicondo ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Multiple Reaction Monitoring ◽  
Screening Method ◽  
Simultaneous Detection ◽  
Forensic Toxicology ◽  
Analytical Sensitivity ◽  
New Psychoactive Substance ◽  
Wide Range ◽  
Drugs In Blood ◽  
Time Resource

In the last few years, liquid chromatography coupled with mass spectrometry (LC/MS) has been increasingly used for screening purposes in forensic toxicology. These techniques have the advantages of low time/resource-consuming and high versatility and have been applied in numerous new multi-analytes methods. The new psychoactive substance (NPS) phenomenon provided a great impulse to this wide-range approach, but it is also important to keep the attention on “classical” psychoactive substances, such as benzodiazepines (BDZ). In this paper, a fully validated screening method in blood for the simultaneous detection of 163 substances (120 NPS and 43 other drugs) by a dynamic multiple reaction monitoring analysis through LC-MS/MS is described. The method consists of a deproteinization of 200 µL of blood with acetonitrile. The LC separation is achieved with a 100 mm long C18 column in 35 min. The method was very sensitive, with limits of quantification from 0.02 to 1.5 ng/mL. Matrix effects did not negatively affect the analytical sensitivity. This method proved to be reliable and was successfully applied to our routinary analytical activity in several forensic caseworks, allowing the identification and quantification of many BDZs and 3,4-methylenedioxypyrovalerone (MDPV).

scholarly journals New Psychoactive Substances: A Matter of Time

2019 ◽  
Vol 17 (9) ◽  
pp. 818-822 ◽  
Author(s):  
Flaminia Pantano ◽  
Silvia Graziano ◽  
Roberta Pacifici ◽  
Francesco Paolo Busardò ◽  
Simona Pichini
Keyword(s):  
Mechanism Of Action ◽  
Early Warning ◽  
Early Warning System ◽  
Time Lag ◽  
Warning System ◽  
Screening Tests ◽  
New Psychoactive Substances ◽  
Psychoactive Substances ◽  
Poor Knowledge ◽  
Wide Range

In the last few years, a wide range of new psychoactive substances (NPS) have been produced and marketed to elude the controlled substance lists. These molecules enter the traditional illegal and web market with poor knowledge about their toxicity, mechanism of action, metabolism, abuse potential so that they are directly tested by the consumers. This perspective highlights the main issues connected with NPS: the celerity they enter and leave the market once included in the banning laws to be substituted by new legal analogues; the unavailability of analytical screening tests and certified standards to perform toxicological analyses; the time lag between NPS identification and inclusion in the controlled substances lists. Finally, the authors take a snapshot of the commitment of the Italian Early Warning System in highlighting the recent seizures of NPS as well as the distribution of NPS related intoxication and deaths as an example of what is happening in the European countries and internationally.

scholarly journals Molecular Networking: A Useful Tool for the Identification of New Psychoactive Substances in Seizures by LC–HRMS

2020 ◽  
Vol 8 ◽  
Author(s):  
Flaminia Vincenti ◽  
Camilla Montesano ◽  
Francesca Di Ottavio ◽  
Adolfo Gregori ◽  
Dario Compagnone ◽  
...  
Keyword(s):  
Natural Product ◽  
Illicit Drugs ◽  
Synthetic Cannabinoids ◽  
New Psychoactive Substances ◽  
Nmr Analysis ◽  
Psychoactive Substances ◽  
Molecular Networking ◽  
Fentanyl Analogs ◽  
Global Concern ◽  
Product Search

New Psychoactive Substances (NPS) are a global concern since they are spreading at an unprecedented rate. Despite their commerce still being limited compared to traditional illicit drugs, the identification of NPS in seizures may represent a challenge because of the variety of possible structures. In this study we report the successful application of molecular networking (MN) to identify unexpected fentanyl analogs in two seizures. The samples were extracted with 1 mL of methanol and analyzed with an untargeted data-dependent acquisition approach by LC–HRMS. The obtained data were examined using the MN workflow within the Global Natural Product Search (GNPS). A job was submitted to GNPS by including both seizures and standard mixtures containing synthetic cannabinoids and fentanyls raw files; spectra obtained from standards were used to establish representative networks for both molecular classes. All synthetic cannabinoids in the mixture were linked together resulting in a molecular network despite their different fragmentation spectra. Looking at fentanyls, all the molecules with the typical 188.143 and 105.070 fragments were combined in a representative network. By exploiting the standard networks two unexpected fentanyls were found in the analyzed seizures and were putatively annotated as para-fluorofuranylfentanyl and (iso)butyrylfentanyl. The identity of these two fentanyl analogs was confirmed by NMR analysis. Other m/z ratios in the seizures were compatible with fentanyl derivatives; however, they appeared to be minor constituents, probably impurities or synthetic byproducts. The latter might be of interest for investigations of common fingerprints among different seizures.

Recent bionalytical methods for the determination of new psychoactive substances in biological specimens

Bioanalysis ◽  
2020 ◽  
Vol 12 (21) ◽  
pp. 1557-1595
Author(s):  
Ana Y Simão ◽  
Mónica Antunes ◽  
Hernâni Marques ◽  
Tiago Rosado ◽  
Sofia Soares ◽  
...  
Keyword(s):  
Acute Toxicity ◽  
Analytical Methods ◽  
Synthetic Cannabinoids ◽  
New Psychoactive Substances ◽  
Screening Methods ◽  
Psychoactive Substances ◽  
Clinical Action ◽  
One Step ◽  
Preparation Techniques

One of the problems associated with the consumption of new psychoactive substances is that in most scenarios of acute toxicity the possibility of quick clinical action may be impaired because many screening methods are not responsive to them, and laboratories are not able to keep pace with the appearance of new substances. For these reasons, developing and validating new analytical methods is mandatory in order to efficiently face those problems, allowing laboratories to be one step ahead. The goal of this work is to perform a critical review regarding bionalytical methods that can be used for the determination of new psychoactive substances (phenylethylamines, cathinones, synthetic cannabinoids, opioids, benzodiazepines, etc), particularly concerning sample preparation techniques and associated analytical methods.

scholarly journals Streets of the ‘spice zombies’: Dependence and poverty stigma in times of austerity

2019 ◽  
Vol 16 (1) ◽  
pp. 97-113 ◽  
Author(s):  
Liviu Alexandrescu
Keyword(s):  
Synthetic Cannabinoids ◽  
Public Spaces ◽  
Cultural Analysis ◽  
New Psychoactive Substances ◽  
The Political ◽  
Psychoactive Substances ◽  
Political Discourses ◽  
The United Kingdom ◽  
The Poor ◽  
National Media

Following the 2016 general ban on new psychoactive substances, synthetic cannabinoids (‘spice’-type drugs) have moved into unregulated street markets and have become popular among homeless populations in the United Kingdom. Images of so-called ‘spice zombies’, rough sleepers in public spaces experiencing severe substance-induced fits, have been used by local and national media to suggest the growing scale of the problem. This article proposes that such depictions should be read through a cultural analysis rooted in the political economy of austerity policies, where the twofold stigma of substance and welfare dependencies directs guilt at the poor, concealing the systemic cruelty of benefits reforms. Through the circulation of such tropes and the ridiculing of a superfluous abject underclass that embodies them, media and political discourses of the ‘broken society’ highlight an evident need for welfare reduction and more generally for the austerity project.

Oral fluid drug analysis in the age of new psychoactive substances

Bioanalysis ◽  
2016 ◽  
Vol 8 (7) ◽  
pp. 691-710 ◽  
Author(s):  
Elisabeth Leere Øiestad ◽  
Åse Marit Leere Øiestad ◽  
Astrid Gjelstad ◽  
Ritva Karinen
Keyword(s):  
Oral Fluid ◽  
Drug Analysis ◽  
New Psychoactive Substances ◽  
Psychoactive Substances

MT-45: A new, dangerous legal high

2014 ◽  
Vol 10 (5) ◽  
pp. 301 ◽  
Author(s):  
Maurizio Coppola, MD ◽  
Raffaella Mondola, MD
Keyword(s):  
Prescription Drugs ◽  
Synthetic Cannabinoids ◽  
Epidemiological Data ◽  
New Psychoactive Substances ◽  
Psychoactive Substances ◽  
Legal Highs ◽  
Smart Drugs ◽  
Research Chemicals ◽  
Medical Emergencies ◽  
Legal High

Epidemiological data confirm that the use of new psychoactive substances is on the rise around the world.1 Numerous reports have described medical emergencies associated with the consumption of unconventional drugs of misuse bought in “head” or “smart” shops or online.1 New psychoactive substances, also referred as “legal highs,” “smart drugs,” or “research chemicals,” are a large group of both plant derivatives and synthetic compounds, also in combination, purposefully designed as legal alternatives to illicit substances of abuse. The most popular and widely-spread new psychoactive substances are synthetic cannabinoids and synthetic cathinones, however, various different compounds such as amphetamine-like molecules, arylcyclohexylamines, synthetic hallucinogens, prescription drugs and hormones have been found in recreational products marketed as legal highs.1

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