Detection and Quantification of 56 New Psychoactive Substances in Whole Blood and Urine by LC–MS/MS

Ambach, Lars; Redondo, Ana Hernández; König, S.; Angerer, Verena; Schürch, Stefan; Weinmann, Wolfgang

doi:10.4155/bio.15.48

Cited by 40 publications

(16 citation statements)

References 68 publications

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“…In consideration of these facts, the inclusion of substances with ‘a similar chemical structure or similar biological effect’ as defined in WADA's Prohibited List is an appropriate means of covering the most relevant new additions to the market; however, the identification of novel compounds and characterization of their structures is required in all affected disciplines such as forensic, toxicological, and anti‐doping sciences. Hence, numerous approaches were utilized to characterize and rapidly analyze phenethylamine and cathinone derivatives including ultrahigh performance liquid chromatography (UHPLC) and CE, ion mobility, and MS‐based approaches, upon which comprehensive detection methods have been established for clinical and forensic applications enabling the identification of these compounds and respective degradation products in metabolism studies, blood, and urine . Employing LC‐MS/MS, screening methods for 40 and 56 analytes were developed, which allowed for LODs for urine samples between 1 and 10 ng/mL for all measurands.…”

Section: Stimulantsmentioning

confidence: 99%

“…Hence, numerous approaches were utilized to characterize and rapidly analyze phenethylamine and cathinone derivatives including ultrahigh performance liquid chromatography (UHPLC) and CE, [189] ion mobility, [190,191] and MS-based approaches, upon which comprehensive detection methods have been established for clinical and forensic applications enabling the identification of these compounds and respective degradation products in metabolism studies, blood, and urine. [192][193][194] Employing LC-MS/MS, screening methods for 40 and 56 analytes were developed, which allowed for LODs for urine samples between 1 and 10 ng/mL for all measurands. Alternatively, albeit not tested for as many analytes, the use of direct analysis in real time (DART)-MS with and without solid-phase microextraction (SPME) employing custom-made extraction fibers and sample holders was presented.…”

Section: Stimulantsmentioning

confidence: 99%

“…--2 Diuretics - [182] --S6 Stimulants [63,191,203,205] [189,[192][193][194][196][197][198][199][200]202,204] [24, [186][187][188][189][190][191]195,198,201] S7 Narcotics ----S8 Cannabinoids [208][209][210] [ 95,[208][209][210][211][212][214][215][216][217] - [206][207][208][209][210]213,216] S9 Glucocorticosteroids - [221][222][223][224][225] - [24,...…”

Section: Introductionunclassified

See 2 more Smart Citations

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis

Kuuranne

Walpurgis

et al. 2016

Drug Testing and Analysis

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The aim of improving anti-doping efforts is predicated on several different pillars, including, amongst others, optimized analytical methods. These commonly result from exploiting most recent developments in analytical instrumentation as well as research data on elite athletes' physiology in general, and pharmacology, metabolism, elimination, and downstream effects of prohibited substances and methods of doping, in particular. The need for frequent and adequate adaptations of sports drug testing procedures has been incessant, largely due to the uninterrupted emergence of new chemical entities but also due to the apparent use of established or even obsolete drugs for reasons other than therapeutic means, such as assumed beneficial effects on endurance, strength, and regeneration capacities. Continuing the series of annual banned-substance reviews, literature concerning human sports drug testing published between October 2014 and September 2015 is summarized and reviewed in reference to the content of the 2015 Prohibited List as issued by the World Anti-Doping Agency (WADA), with particular emphasis on analytical approaches and their contribution to enhanced doping controls.

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Section: Stimulantsmentioning

confidence: 99%

Section: Stimulantsmentioning

confidence: 99%

See 1 more Smart Citation

Annual banned‐substance review: analytical approaches in human sports drug testing

Thevis

Kuuranne

Walpurgis

et al. 2016

Drug Testing and Analysis

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show abstract

“…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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“…At present, liquid chromatography–tandem mass spectrometry (LC/MS/MS) is by far the most frequently used method for screening and confirmation of some new emerging variant NPSs because of its high sensitivity, selectivity, and capability of providing further structural information about these molecules . High‐resolution and high‐accuracy mass spectrometry can provide more sensitive results and full spectral data with high mass accuracy and resolution.…”

mentioning

confidence: 99%

Rapid screening and determination of 11 new psychoactive substances by direct analysis in real time mass spectrometry and liquid chromatography/quadrupole time‐of‐flight mass spectrometry

Hua

Pan

et al. 2016

Rapid Comm Mass Spectrometry

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RATIONALE:With the amounts and types of new psychoactive substances (NPSs) increasing rapidly in recent years, an excellent high-throughput method for the analysis of these compounds is urgently needed. In this article, a rapid screening method and a quantitative analysis method for 11 NPSs are described and compared, respectively. METHOD: A simple direct analysis in real time mass spectrometry (DART-MS) method was developed for the analysis of 11 NPSs including three categories of these substances present on the global market such as four cathinones, one phenylethylamine, and six synthetic cannabinoids. In order to analyze these compounds quantitatively with better accuracy and sensitivity, another rapid analytical method with a low limit of detection (LOD) was also developed using liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (LC/QTOFMS). RESULTS: The 11 NPSs could be determined within 0.5 min by DART-MS. Furthermore, they could also be separated and determined within 5 min by the LC/QTOFMS method. The two methods both showed good linearity with correlation coefficients (r 2 ) higher than 0.99. The LODs for all these target NPSs by DART-MS and LC/QTOFMS ranged from 5 to 40 ng mL À1 and 0.1 to 1 ng mL À1 , respectively. Confiscated samples, named as "music vanilla" and "bath salt", and 11 spiked samples were firstly screened by DART-MS and then determined by LC/QTOFMS. CONCLUSIONS: The identification of NPSs in confiscated materials was successfully achieved, and the proposed analytical methodology could offer rapid screening and accurate analysis results.

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Detection and Quantification of 56 New Psychoactive Substances in Whole Blood and Urine by LC–MS/MS

Abstract: A novel method is presented for the unambiguous identification and quantification of 56 NPS in blood and urine samples in clinical and forensic cases, e.g., intoxications or driving under the influence of drugs.

Cited by 40 publications

References 68 publications

Annual banned‐substance review: analytical approaches in human sports drug testing

Annual banned‐substance review: analytical approaches in human sports drug testing

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

Rapid screening and determination of 11 new psychoactive substances by direct analysis in real time mass spectrometry and liquid chromatography/quadrupole time‐of‐flight mass spectrometry

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