Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry

Lehmann, Sabrina; Kieliba, Tobias; Beike, Justus; Thevis, Mario; Mercer‐Chalmers‐Bender, Katja

doi:10.1016/j.jchromb.2017.09.003

Cited by 45 publications

(24 citation statements)

References 31 publications

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“…The LC−ESI−MS/MS method development was based on the earlier study on the determination of NPS by Lehmann et al utilizing the same stationary and mobile phase. The authors used a Kinetex Core‐Shell Biphenyl column for chromatographic separation ─ a column not only recommended for use with NPS, but also for the separation of synthetic cannabinoid metabolites .…”

Section: Resultsmentioning

confidence: 99%

“…The authors used a Kinetex Core‐Shell Biphenyl column for chromatographic separation ─ a column not only recommended for use with NPS, but also for the separation of synthetic cannabinoid metabolites . In addition, the following parameters were maintained: flow rate, column temperature, and the mobile phase, consisting of ammonium formate buffer and ACN, both acidified with 0.1% HCOOH, a combination frequently described in the literature . Variation of the flow rate (to 0.5 mL/min, 0.6 mL/min, and 0.8 mL/min), as well as a variation of the column oven temperature (to 50°C and 60°C), did not influence the separation or the peak symmetry.…”

Section: Resultsmentioning

confidence: 99%

“…Variation of the flow rate (to 0.5 mL/min, 0.6 mL/min, and 0.8 mL/min), as well as a variation of the column oven temperature (to 50°C and 60°C), did not influence the separation or the peak symmetry. However, utilizing the gradient with an initial solvent B proportion of 10% led to both a very late and incomplete elution of the tested synthetic cannabinoid metabolites from the column. As a result, further optimization was needed, which was based on a published gradient elution starting with 40% of solvent B (0.01% HCOOH in MeOH/ACN (v/v = 50/50)) and increasing to a maximum of 98% within 9.5 minutes .…”

Section: Resultsmentioning

confidence: 99%

“…Optimization of the ESI source parameters, with the exception of the sheath gas flow, which was set to 12 L/min, was made on previously published settings . In six test series, three measurements were conducted for each parameter while maintaining the remaining parameters: capillary voltage, gas temperature, nebulizer, sheath gas temperature, gas flow, and nozzle voltage.…”

Section: Resultsmentioning

confidence: 99%

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Solid‐phase extraction–liquid chromatography–tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine

Gaunitz

Kieliba

Thevis

et al. 2019

Drug Testing and Analysis

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This article comprises the development and validation of a protocol for the qualitative analysis of 61 phase I synthetic cannabinoid metabolites in urine originating from 29 synthetic cannabinoids, combining solid‐phase extraction (SPE) utilizing a reversed phase silica‐based sorbent (phenyl) with liquid chromatography–tandem mass spectrometry (LC−MS/MS). Validation was performed according to the guidelines of the German Society of Toxicological and Forensic Chemistry. Sufficient chromatographic separation was achieved within a total runtime of 12.3 minutes. Validation included specificity and selectivity, limit of detection (LOD), recovery and matrix effects, as well as auto‐sampler stability of processed urine samples. LOD ranged between 0.025 ng/mL and 0.5 ng/mL in urine. Recovery ranged between 43% and 97%, with only two analytes exhibiting recoveries below 50%. However, for those two analytes, the LODs were 0.05 ng/mL in urine. In addition, matrix effects between 81% and 185% were determined, whereby matrix effects over 125% were observed for 10 non‐first‐generation synthetic cannabinoid metabolites. The developed method enables the rapid and sensitive detection of synthetic cannabinoid metabolites in urine, complementing the spectrum of existing analytical tools in forensic case work. Finally, application to 61 urine samples from both routine and autopsy case work yielded one urine sample that tested positive for ADB‐PINACA N‐pentanoic acid.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

See 2 more Smart Citations

Solid‐phase extraction–liquid chromatography–tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine

Gaunitz

Kieliba

Thevis

et al. 2019

Drug Testing and Analysis

Self Cite

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“…On the other hand, NPS were determined in biological matrixes, such as serum [19,20,28,29], blood [21][22][23], urine [21,[24][25][26][27], oral fluid [28], as well as in hair [29] by LC-MS/MS [30].…”

Section: Introductionmentioning

confidence: 99%

Separation of enantiomers of new psychoactive substances by high‐performance liquid chromatography

Kadkhodaei

Forcher

Schmid

2018

J of Separation Science

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New psychoactive substances are defined as compounds with consciousness-changing effects and have been developed simultaneously with classical drugs. They arise through structural modifications of illegal substances and are mainly produced to circumvent laws. Availability is simple, since new psychoactive substances can be purchased from the Internet. Among them many chemical drug compound classes are chiral and thus the two resulting enantiomers can differ in their effects. The aim of this study is to develop a suitable chiral high-performance liquid chromatography separation method for a broad spectrum of new psychoactive substances using cellulose tris(3,5-dichlorophenylcarbamate) as a chiral selector. Experiments were performed by high-performance liquid chromatography in normal-phase mode under isocratic conditions using ultraviolet detection. Direct separation was carried out on a high-performance liquid chromatography column (Lux® i-Cellulose-5, 3.5 μm, Phenomenex®), available since 2016. Excellent separation results were obtained for cathinones. After further optimization, even 47 instead of 39 out of 52 cathinones showed baseline separation. For amphetamine derivatives, satisfactory results were not achieved. Further, new psychoactive substances from other compound classes such as benzofuranes, thiophenes, phenidines, phenidates, morpholines, and ketamines were partially resolved, depending on the polarity and degree of substitution. All analytes, which were mainly purchased from the Internet, were proven to be traded as racemates.

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Aspects of Sample Preparation

2020

Fundamentals of Analytical Toxicology

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Determination of 74 new psychoactive substances in serum using automated in-line solid-phase extraction-liquid chromatography-tandem mass spectrometry

Cited by 45 publications

References 31 publications

Solid‐phase extraction–liquid chromatography–tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine

Solid‐phase extraction–liquid chromatography–tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine

Separation of enantiomers of new psychoactive substances by high‐performance liquid chromatography

Aspects of Sample Preparation

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