LC–MS/MS and volumetric absorptive microsampling for quantitative bioanalysis of cathinone analogues in dried urine, plasma and oral fluid samples

Mercolini, Laura; Protti, Michele; Catapano, Maria Carmen; Rudge, James; Sberna, Angelo Eliseo

doi:10.1016/j.jpba.2016.02.015

Cited by 100 publications

(47 citation statements)

References 30 publications

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“…The extraction step is usually carried out on DMS with a suitable solvent and the resulting sample can be injected as such. Alternatively, the extract can be subjected to further clean‐up steps . In this case, solvent nature and volume were the only tested parameters, obtaining comparable results from both DMS matrices: pure methanol proved to be the most efficient extractor, while also granting satisfactory purification from matrix interference.…”

Section: Resultsmentioning

confidence: 99%

Enantioseparation and determination of asenapine in biological fluid micromatrices by HPLC with diode array detection

Protti

Vignali

Blanco

et al. 2018

J of Separation Science

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Asenapine is a recent drug approved in the European Union for the treatment of bipolar disorder. An original approach has been developed for asenapine analysis in patients treated with the drug, including miniaturized microsampling procedures, separation and quantitation of drug enantiomers. An original enantioselective method based on high-performance liquid chromatography with diode array detection was developed and applied to the determination of asenapine enantiomer levels in innovative haematic samples: four micromatrices have been tested, two based on dried matrix spots (dried blood spots and dried plasma spots) and two based on volumetric absorptive microsampling (from blood and plasma). Chiral separation was achieved on a cellulose-tris(3,5 dimethylphenylcarbamate) column, with a mobile phase containing bicarbonate buffer and acetonitrile. The method was validated with satisfactory results of linearity and precision on all matrices that showed also a significant performance in terms of stability, feasibility and reliability, when compared to fluid plasma sampling, handling and processing. Among micromatrices, both volumetric absorptive microsampling types were superior to dried matrix spots in terms of data reproducibility and correspondence with plasma levels. The bioanalytical approach proposed herein provides for the first time a chiral high-performance liquid chromatographic method for the determination of asenapine enantiomers, coupled to a very effective microsampling strategy.

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Section: Resultsmentioning

confidence: 99%

Enantioseparation and determination of asenapine in biological fluid micromatrices by HPLC with diode array detection

Protti

Vignali

Blanco

et al. 2018

J of Separation Science

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“…As an alternative to pipetting defined volumes of blood on DBS cards, the technique of volumetric absorptive microsampling was shown to provide reproducible and accurate results. As illustrated with dried urine, plasma, and oral fluid, six model cathinone analogues were detected in 10 μL specimens sampled by saturation of an absorptive tip, followed by LC‐MS/MS analysis …”

Section: Stimulantsmentioning

confidence: 99%

“…As illustrated with dried urine, plasma, and oral fluid, six model cathinone analogues were detected in 10 μL specimens sampled by saturation of an absorptive tip, followed by LC-MS/MS analysis. [144] Narcotics and glucocorticoids Anti-doping rule violations (ADRVs) in connection with narcotics have become comparably rare phenomena. Nevertheless, since these compounds constitute a class of prohibited substances of the WADA Prohibited List, [26] test methods enabling the qualitative and, in case of morphine, [70] quantitative determination of relevant analytes are required.…”

Section: Stimulantsmentioning

confidence: 99%

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

Thevis

Kuuranne

Geyer

et al. 2017

Drug Testing and Analysis

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There has been an immense amount of visibility of doping issues on the international stage over the past 12 months with the complexity of doping controls reiterated on various occasions. Hence, analytical test methods continuously being updated, expanded, and improved to provide specific, sensitive, and comprehensive test results in line with the World Anti-Doping Agency's (WADA) 2016 Prohibited List represent one of several critical cornerstones of doping controls. This enterprise necessitates expediting the (combined) exploitation of newly generated information on novel and/or superior target analytes for sports drug testing assays, drug elimination profiles, alternative test matrices, and recent advances in instrumental developments. This paper is a continuation of the series of annual banned-substance reviews appraising the literature published between October 2015 and September 2016 concerning human sports drug testing in the context of WADA's 2016 Prohibited List. Copyright © 2016 John Wiley & Sons, Ltd.

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“…24 Recent proposals also perform direct determination (chromatographic injection) after protein separation by centrifugation, 26-28 enzymatic hydrolysis and centrifugation, 29,30 conventional (available commercial cartridges) SPE, [31][32][33][34][35] and LLE. [36][37][38][39][40][41][42] Finally, solid-phase microextraction (SPME), 43 and volumetric absorptive microsampling (VAMS) 44 have been also used for cathinones assessment in urine. Some of these developments deal with the assessment of a specific synthetic cathinone, such as 3,4-dimethylmethcathinone (3,4-DMMC), 29 4′-methyl-α-pyrrolidinohexanophenone (MPHP), 27 3,4methylenedioxypyrovalerone (MDPV), 41 mephedrone, 42 and metabolic profiles regarding pyrrolidinohexiophenone (α-PHP), 39 1-phenyl-2-(1-pyrrolidinyl)-1-heptanone (PV8), 34 and 1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one (α-PVP).…”

Section: Introductionmentioning

confidence: 99%

“…40 However, appealing methodologies should be applicable to the simultaneous extraction of synthetic cathinones. Some examples of simultaneous assessment of synthetic cathinones 28,32,35,37,38,43,44 and synthetic cathinones and other NPS classes 25,26,30,31,33,36 can also be found in the literature.…”

Section: Introductionmentioning

confidence: 99%

HPLC‐MS/MS combined with membrane‐protected molecularly imprinted polymer micro‐solid‐phase extraction for synthetic cathinones monitoring in urine

Sánchez–González

Odoardi

Bermejo

et al. 2018

Drug Testing and Analysis

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Synthetic cathinones are a type of drug belonging to group of new psychoactive substances (NPSs). The illicit market for these substances is characterized by the continuous introduction to the market of new analogs to evade legislation and to avoid detection. New screening and confirmation assays are therefore needed, mainly in forensic/clinical samples. In the current development, a porous membrane-protected, micro-solid-phase extraction (μ-SPE) has been developed for the assessment of several cathinones in urine. The μ-SPE device consisted of a cone-shaped polypropylene (PP) porous membrane containing the adsorbent (molecularly imprinted polymers, MIPs, synthesized for the first time for this class of drugs). MIPs were prepared using ethylone and 3-methylmethcathinone (3-MMC) as templates, ethylene glycol dimethacrylate (EGDMA) as a functional monomer, divinylbenzene (DVB) as a cross-linker, and 2,2´-azobisisobutyronitrile (AIBN) as an initiator. The prepared ethylone-based MIP and 3-MMC-based MIP have been fully characterized and evaluated as new selective adsorbents for μ-SPE. Cathinones separation/determination was performed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Optimum loading conditions (pH 5.0, loading for 4.0 minutes under orbital-horizontal shaking at 200 rpm) and elution conditions [2.0 mL of 75:20:5 heptane/2-propanol/ammonium hydroxide and ultrasounds assistance (37 kHz, 325 W) for 4.0 minutes] were found for ethylone-based MIP. Validation (intra-day and inter-day precision and analytical recovery) showed RSD values lower than 9 and 10% for intra-day and inter-day precision, and within the 88%-101% range for intra-day and inter-day analytical recovery.

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LC–MS/MS and volumetric absorptive microsampling for quantitative bioanalysis of cathinone analogues in dried urine, plasma and oral fluid samples

Cited by 100 publications

References 30 publications

Enantioseparation and determination of asenapine in biological fluid micromatrices by HPLC with diode array detection

Enantioseparation and determination of asenapine in biological fluid micromatrices by HPLC with diode array detection

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

HPLC‐MS/MS combined with membrane‐protected molecularly imprinted polymer micro‐solid‐phase extraction for synthetic cathinones monitoring in urine

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