Identification and quantification of synthetic cathinones in blood and urine using liquid chromatography-quadrupole/time of flight (LC-Q/TOF) mass spectrometry

Glicksberg, Lindsay; Bryand, Kelsie; Kerrigan, Sarah

doi:10.1016/j.jchromb.2016.09.027

Cited by 65 publications

(35 citation statements)

References 24 publications

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“…For blood, sample preparation procedures included protein precipitation, liquid-liquid extraction (LLE), salting-out assisted liquid-liquid extraction (SALLE) and microwaveassisted extraction (MAE) [28][29][30][31][32]. Glicksberg et al [28] reported the use of protein precipitation with acetonitrile followed by solid-phase extraction (SPE) for the extraction of synthetic cathinones from blood plasma and urine.…”

Section: Biological Matricesmentioning

confidence: 99%

“…Glicksberg et al [28] reported the use of protein precipitation with acetonitrile followed by solid-phase extraction (SPE) for the extraction of synthetic cathinones from blood plasma and urine. Extraction efficiencies of greater than 80% and 90% were reported for plasma and urine, respectively.…”

Section: Biological Matricesmentioning

confidence: 99%

“…LC has been the most commonly adopted conventional separation technique coupled to HRMS for the analysis of NPS due to the well-recognized fact that analytes of interest do not need to be volatile and do not require derivatization [15,28,30,33,39,42,43,[46][47][48].…”

Section: Conventional Separation Techniques Coupled To Hrmsmentioning

confidence: 99%

“…Additionally, DDA can be operated in a targeted precursor selection mode whereby MS/MS events are triggered when pre-selected mass-to-charge (m/z) ratios in inclusions lists are detected in the preceding MS scan [28,45,49]. These inclusion lists are typically populated with precursor ion data and, if known, retention times obtained from CRMs.…”

Section: Direct Sample Analysis Techniques Coupled To Hrmsmentioning

confidence: 99%

See 3 more Smart Citations

Current applications of high-resolution mass spectrometry for the analysis of new psychoactive substances: a critical review

Pasin

Cawley

Bidny³

et al. 2017

Anal Bioanal Chem

112

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The proliferation of new psychoactive substances (NPS) in recent years has resulted in the development of numerous analytical methods for the detection and identification of known and unknown NPS derivatives. High-resolution mass spectrometry (HRMS) has been identified as the method of choice for broad screening of NPS in a wide range of analytical contexts due to its ability to measure accurate masses using data-independent acquisition (DIA) techniques. Additionally, it has shown promise for non-targeted screening strategies that have been developed in order to detect and identify novel analogues without the need for certified reference materials (CRMs) or comprehensive mass spectral libraries. This paper reviews the applications of HRMS for the analysis of NPS in forensic drug chemistry, clinical and forensic toxicology. It provides an overview of the sample preparation procedures in addition to data acquisition, instrumental analysis and data processing techniques.Furthermore, it will give an overview of the current state of non-targeted screening strategies with discussion on future directions and perspectives of this technique.3

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Section: Biological Matricesmentioning

confidence: 99%

Section: Biological Matricesmentioning

confidence: 99%

Section: Conventional Separation Techniques Coupled To Hrmsmentioning

confidence: 99%

Section: Direct Sample Analysis Techniques Coupled To Hrmsmentioning

confidence: 99%

See 2 more Smart Citations

Current applications of high-resolution mass spectrometry for the analysis of new psychoactive substances: a critical review

Pasin

Cawley

Bidny³

et al. 2017

Anal Bioanal Chem

112

View full text Add to dashboard Cite

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“…A significant increase in the abuse of synthetic cathinones (the β-keto analogues of amphetamine) has been reported. [77][78][79][80] Cathinone is the main psychoactive element of Khat (Cathis edulis), chewing the leaves of which is used for treatment of respiratory conditions due to relaxation of airway smooth muscle and, thus, it may be considered as an instant substitute for clenbuterol in racehorses. Psychostimulating and hallucinogenic properties are also attributed to cathinones.…”

Section: (Designer) Stimulants and Opioidsmentioning

confidence: 99%

Challenges in detecting substances for equine anti‐doping

Fragkaki

Kioukia‐Fougia

Kiousi

et al. 2017

Drug Testing and Analysis

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The artificial increase of the physical capability of horses using drugs is well known in racing and other equine sports. Both illicit and therapeutic substances are regarded as prohibited substances in competition in most countries. Some countries make distinctions for a few, specific drugs which are, however, allowed for use in other countries. The primary objective in the case of doping control is the detection of any trace of drug exposure, either parent drug or any of its metabolites, using the most powerful analytical methods which are generally based on chromatographic/mass spectrometric techniques. Of major concern in horseracing is the absence of a single organization regulating the anti-doping framework; instead of this, individual racing authorities provide rules and regulations often resulting in variations in the applied doping control programmes of different countries. The aim of this paper is to review the recent literature (approximately from 2012 to mid-2016) to highlight the numerous and diverse challenges faced in doping control of racing and equestrian sports, including the detection of designer drugs (anabolic steroids or stimulants) and of other emerging prohibited substances, such as peptides and noble gases in horse urine and plasma. Moreover, the application of 'omics' techniques (especially of metabolomics) deserves attention for establishing possible fingerprints of drug abuse as well as the evolution of instrumental analysis resulting a powerful ally in the fight against doping in equine sports.

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Study of the in vitro and in vivo metabolism of the tryptamine 5‐MeO‐MiPT using human liver microsomes and real case samples

Grafinger

Hädener

König

et al. 2017

Drug Testing and Analysis

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The synthetic tryptamine 5-methoxy-N-methyl-N-isopropyltryptamine (5-MeO-MiPT) has recently been abused as a hallucinogenic drug in Germany and Switzerland. This study presents a case of 5-MeO-MiPT intoxication and the structural elucidation of metabolites in pooled human liver microsomes (pHLM), blood, and urine. Microsomal incubation experiments were performed using pHLM to detect and identify in vitro metabolites. In August 2016, the police encountered a naked man, agitated and with aggressive behavior on the street. Blood and urine samples were taken at the hospital and his premises was searched. The obtained blood and urine samples were analyzed for in vivo metabolites of 5-MeO-MiPT using LC-high resolution MS/MS (LC-HR-MS/MS). The confiscated pills and powder samples were qualitatively analyzed using FTIR, GC-MS, LC-HR-MS/MS and NMR. 5-MeO-MiPT was identified in two of the seized powder samples. General unknown screening detected cocaine, cocaethylene, methylphenidate, ritalinic acid and 5-MeO-MiPT in urine. Seven different in vitro phase I metabolites of 5-MeO-MiPT were identified. In the forensic case samples, four phase I metabolites could be identified in blood and seven in urine. The five most abundant metabolites were formed by demethylation and hydroxylation of the parent compound. 5-MeO-MiPT concentrations in the blood and urine sample were found to be 160 ng/mL and 3380 ng/mL, respectively. Based on the results of this study we recommend metabolites 5-methoxy-Nisopropyltryptamine (5-MeO-NiPT), 5-hydroxy-N-methyl-N-isopropyltryptamine (5-OH-MiPT), 5-methoxy-N-methyl-N-isopropyltryptamine-N-oxide (5-MeO-MiPT-N-oxide) and hydroxy-5-methoxy-N-methyl-N-isopropyltryptamine (OH-5-MeO-MiPT) as biomarkers for the development of new methods for the detection of 5-MeO-MiPT consumption, as they have been present in both blood and urine samples.

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Identification and quantification of synthetic cathinones in blood and urine using liquid chromatography-quadrupole/time of flight (LC-Q/TOF) mass spectrometry

Cited by 65 publications

References 24 publications

Current applications of high-resolution mass spectrometry for the analysis of new psychoactive substances: a critical review

Current applications of high-resolution mass spectrometry for the analysis of new psychoactive substances: a critical review

Challenges in detecting substances for equine anti‐doping

Study of the in vitro and in vivo metabolism of the tryptamine 5‐MeO‐MiPT using human liver microsomes and real case samples

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