Screening of Novel Psychoactive Substances in Postmortem Matrices by Liquid Chromatography–Tandem Mass Spectrometry (LC–MS-MS)†

Fagiola, Michael; Hahn, Timothy; Avella, Joseph

doi:10.1093/jat/bky050

Cited by 36 publications

(24 citation statements)

References 16 publications

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“…The production of fragments from ethylone signal, m/z 222.1127, 21 Figure 4A, is based on the mass loss of 45 Da attributed to the elimination of NH 2 CH 2 CH 3 assisted by the β‐hydrogen removal resulting in the signal at m/z 177.0547. Otherwise, a rearrangement of the 1,3‐methyl shift to the protonated carbonyl group leads to the release of water with mass loss of 18 Da attributed to the ion at m/z 204.1021 followed by the elimination process of methoxyl group (30 Da) at the phenyl moiety corresponding to the signal with m/z 174.0915 54 . Besides, the fragment at m/z 204.1021 can generate the ion at m/z 176.0707 due to the release of CH 2 CH 2 (28 Da) assisted by β‐hydrogen removal by the nitrogen atom following the cleavage of N–C bond.…”

Section: Resultsmentioning

confidence: 99%

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Exploring the chemical profile of designer drugs by ESI(+) and PSI(+) mass spectrometry—An approach on the fragmentation mechanisms and chemometric analysis

et al. 2020

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The consumption of design drugs, frequently known as new psychoactive substances (NPS), has increased considerably worldwide, becoming a severe issue for the responsible governmental agencies. These illicit substances can be defined as synthetic compounds produced in clandestine laboratories in order to act as analogs of schedule drugs mimetizing its chemical structure and improving its pharmacological effects while hampering the control and making regulation more complicated. In this way, the development of new methodologies for chemical analysis of NPS drugs is indispensable to determine a novel class of drugs arising from the underground market. Therefore, this work shows the use of high-resolution mass spectrometry Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) applying different ionization sources such as paper spray ionization (PSI) and electrospray ionization (ESI) in the evaluation of miscellaneous of seized drugs samples as blotter paper (n = 79) and tablet (n = 100). Also, an elucidative analysis was performed by ESI(+) MS/MS experiments, and fragmentation mechanisms were proposed to confirm the chemical structure of compounds identified. Besides, the results of ESI(+) and PSI(+)-FT-ICR MS were compared with those of GC-MS, revealing that ESI(+)MS showed greater detection efficiency among the methodologies employed in this study. Moreover, this study stands out as a guide for the chemical analysis of NPS drugs, highlighting the differences between the techniques of ESI(+)-FT-ICR MS, PSI(+)-FT-ICR MS, and GC-MS.

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Section: Resultsmentioning

confidence: 99%

“…52,53 The production of fragments from ethylone signal, m/z 222.1127, 21 Figure 4A, 189.0786. 21,54 Similarly to ethylone, Figure 4A ated by the nitrogen moiety to release benzene followed by the elimination of ammonia to produce the fragment at m/z 165.0468. 58,59 The signal at m/z 329.1188 can be related to the U-47700 compound, Figure S5.…”

Section: Tabletsmentioning

confidence: 99%

Exploring the chemical profile of designer drugs by ESI(+) and PSI(+) mass spectrometry—An approach on the fragmentation mechanisms and chemometric analysis

et al. 2020

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“…To detect the use of NPS, metabolites and/or the parent molecule, is a particular analytical challenge in biofluids, being difficult because of the low concentrations encountered for the more potent substances and the lack of knowledge about many of them (15)(16)(17)(18)(19)(20). Table 2 shows the analytical conditions defined for each substance with the respective detection limits obtained.…”

Section: Limits Of Detectionmentioning

confidence: 99%

Development and validation of a LC-ESI-MS/MS method for simultaneous whole blood analysis of 51 new psychoactive substances

2019

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In recent years, there has been a great increase in seizures and forensic analysis of new psychotropic substances (NPS) in the state of Rio Grande do Sul. The analysis of these compounds needs to be performed in biological samples in cases of violent deaths. A sensitive and reliable liquid chromatography-tandem mass spectrometry with electrospray ionization interface (LC-ESI-MS/MS) method was developed and validated for qualitative analysis of 51 NPS in whole blood forensic samples. Synthetic cathinones, phenethylamines, opioids, tryptamines, synthetic cannabinoids, and other hallucinogens and stimulants were included in the method. The validation parameters assessed were speciﬁcity, limit of detection, retention time precision, and matrix effect. Drug free pools (n=6) were used for validation, including post mortem samples as well as from living individuals. Adulterants, pharmaceuticals, metabolites, and other illicit drugs, totalling 39 compounds, were analyzed and no interference was noticed. The detection limits obtained were suitable for evaluation at recreational and non-fatal levels of consumption, mostly. The results revealed an appropriate matrix effect in 24 out of 51 substances tested, indicating the potential for future quantitative analysis with this method for these drugs. The developed and validated method is easy to implement, fast, with low cost, and suitable for use in routine forensic toxicology laboratory analysis.

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“…28 This also led to the identification of O-desmethylnormethoxetamine and dihydronormethoxetamine. 28 In comparison with the in vitro study, With respect to the knowledge gap on the metabolism of DXE, 42 our study aimed to screen the metabolites in Wistar rat urine samples using liquid chromatography (LC) in combination with high resolution mass spectrometry (HRMS). To fulfil the goal, the most likely major metabolites based on the reported metabolism of the related compounds including the deuterium-labelled standard were synthesized.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and identification of deschloroketamine metabolites in rats' urine and a quantification method for deschloroketamine and metabolites in rats' serum and brain tissue using liquid chromatography tandem mass spectrometry

Hájková

Jurásek

Čejka

et al. 2020

Drug Testing and Analysis

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Deschloroketamine (2‐(methylamino)‐2‐phenyl‐cyclohexanone) is a ketamine analog belonging to a group of dissociative anesthetics, which have been distributed within the illicit market since 2015. However, it was also being sold as ‘ketamine' misleading people to believe that they were getting genuine ketamine. Dissociative anesthetics have also come to the attention of the psychiatric field due to their potential properties in the treatment of depression. At present, there is a dearth of information on deschloroketamine related to its metabolism, biodistribution, and its mechanism of action. We have therefore carried out a metabolomics study for deschloroketamine via non‐targeted screening of urine samples employing liquid chromatography combined with high‐resolution mass spectrometry. We developed and validated a multiple reaction monitoring method using a triple quadrupole instrument to track metabolites of deschloroketamine. Furthermore, significant metabolites of deschloroketamine, (trans‐dihydrodeschloroketamine, cis‐ and trans‐dihydronordeschloroketamine, and nordeschloroketamine), were synthesized in‐house. The prepared standards were utilized in the developed multiple reaction monitoring method. The quantification method for serum samples provided intra‐day accuracy ranging from 86% to 112% with precision of 3% on average. The concentrations of cis/trans‐dihydronordeschloroketamines and trans‐dihydrodeschloroketamine were lower than 10 ng/mL, nordeschloroketamine and deschloroketamine ranged from 0.5 to 860 ng/mL in real samples. The quantification method for brain tissue provided intra‐day accuracy ranging from 80% to 125% with precision of 7% on average. The concentrations of cis/trans‐dihydronordeschloroketamines and trans‐dihydrodeschloroketamine ranged from 0.5 to 70 ng/g, nordeschloroketamine and deschloroketamine varied from 0.5 to 4700 ng/g in real samples.

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Screening of Novel Psychoactive Substances in Postmortem Matrices by Liquid Chromatography–Tandem Mass Spectrometry (LC–MS-MS)†

Cited by 36 publications

References 16 publications

Exploring the chemical profile of designer drugs by ESI(+) and PSI(+) mass spectrometry—An approach on the fragmentation mechanisms and chemometric analysis

Exploring the chemical profile of designer drugs by ESI(+) and PSI(+) mass spectrometry—An approach on the fragmentation mechanisms and chemometric analysis

Development and validation of a LC-ESI-MS/MS method for simultaneous whole blood analysis of 51 new psychoactive substances

Synthesis and identification of deschloroketamine metabolites in rats' urine and a quantification method for deschloroketamine and metabolites in rats' serum and brain tissue using liquid chromatography tandem mass spectrometry

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