Drug Testing and Analysis

Cover image for Vol. 6 Issue 7-8

Early View (Online Version of Record published before inclusion in an issue)

Editor-in-Chief: Prof. Mario Thevis

Impact Factor: 2.816

ISI Journal Citation Reports © Ranking: 2013: 22/76 (Chemistry Analytical); 28/78 (BIOCHEMICAL RESEARCH METHODS); 91/254 (Pharmacology & Pharmacy)

Online ISSN: 1942-7611

VIEW

  1. 1 - 69
  1. Research articles

    1. Performance characteristics of an ELISA screening assay for urinary synthetic cannabinoids

      Eliani Spinelli, Allan J. Barnes, Sheena Young, Marisol S. Castaneto, Thomas M. Martin, Kevin L. Klette and Marilyn A. Huestis

      Article first published online: 28 AUG 2014 | DOI: 10.1002/dta.1702

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      The Neogen SPICE ELISA kit targets JWH-018 N-pentanoic acid as a marker for urinary synthetic cannabinoids. Assay performance was evaluated by analyzing 2469 authentic urine samples with the Neogen immunoassay and liquid chromatography tandem mass spectrometry (LC-MS/MS).The immunoassay was linear from 1–250 µg/L (r2=0.992) with intra- and inter-plate imprecision of ≤5.3% and <9%, respectively. Sensitivity, specificity, and efficiency results with the 5 µg/L cut-off were 79.9%, 99.7%, and 97.4% and with the 10 µg/L cutoff 69.3%, 99.8%, and 96.3%, respectively.

    2. Stable carbon isotope ratio profiling of illicit testosterone preparations – domestic and international seizures

      Lance Brooker, Adam Cawley, Jason Drury, Claire Edey, Nicole Hasick and Catrin Goebel

      Article first published online: 19 AUG 2014 | DOI: 10.1002/dta.1533

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      Stable carbon isotope ratio profiling of illicit testosterone preparations from Australia and abroad has been undertaken to provide up-to-date intelligence for anti-doping laboratories around the world to support the doping control of endogenous anabolic androgenic steroid abuse in human sport.

  2. Correspondence letters

    1. Iron concentration increases after moderate endurance exercise: implications for screening of blood transfusion in sports

      Gian Luca Salvagno, Giuseppe Lippi, Cantor Tarperi, Gian Cesare Guidi and Federico Schena

      Article first published online: 11 AUG 2014 | DOI: 10.1002/dta.1704

  3. Research articles

    1. The use of dried blood spots for quantification of 15 antipsychotics and 7 metabolites with ultra-high performance liquid chromatography - tandem mass spectrometry

      Lisbeth Patteet, Kristof E. Maudens, Christophe P. Stove, Willy E. Lambert, Manuel Morrens, Bernard Sabbe and Hugo Neels

      Article first published online: 31 JUL 2014 | DOI: 10.1002/dta.1698

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      This article describes a UHPLC-MS/MS method for quantification of frequently used antipsychotics and metabolites using dried blood spots. The method was extensively validated, including evaluation of the influence of the hematocrit. The method proved to be a valuable alternative to classical venous blood withdrawal and was evaluated on dried blood spot samples from psychiatric patients.

    2. Test purchase, identification and synthesis of 2-amino-1-(4-bromo-2, 5-dimethoxyphenyl)ethan-1-one (bk-2C-B)

      John D. Power, Pierce Kavanagh, John O'Brien, Michael Barry, Brendan Twamley, Brian Talbot, Geraldine Dowling and Simon D. Brandt

      Article first published online: 30 JUL 2014 | DOI: 10.1002/dta.1699

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      The communication describes the test purchase, identification and synthesis of 2-amino-1-(4-bromo-2,5-dimethoxyphenyl)ethan-1-one (bk-2C-B) a substance recently offered by online vendors of ‘legal highs’ or ‘research chemicals’. Bk-2C-B is the first cathinone derived primary amine, that the authors are aware of, to be marketed.

  4. Short communications

    1. Possibility of analytical finding of glycerol caused by self-catheterization in doping control

      Masato Okano, Yasunori Nishitani and Shinji Kageyama

      Article first published online: 30 JUL 2014 | DOI: 10.1002/dta.1701

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      Glycerol is listed on the prohibited list of the World Anti-Doping Agency as a masking agent because the administration of glycerol increases plasma volume and decreases the concentration of haemoglobin and the value of haematocrit in blood. Self-catheterization is necessary for athletes with neurological disorders such as neurogenic bladder dysfunction. The adverse analytical finding for glycerol for impaired athletes should account for the use of a catheter with glycerol.

  5. Correspondence letters

    1. Cannabis potency in the Venice area (Italy): Update 2013

      Luca Zamengo, Giampietro Frison, Chiara Bettin and Rocco Sciarrone

      Article first published online: 28 JUL 2014 | DOI: 10.1002/dta.1690

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      A significant increase in median values of THC contents was observed in 2013 for both herbal products (+24.6%) and cannabis resin (+9.7%), confirming the previously observed trend (2010-2012) in cannabis potency of seized products in the Venice area (Italy). A significant decreasing trend of the CBD content of cannabis products was also confirmed.

  6. Research articles

    1. Metabolism and urinary disposition of N,N-dimethyltryptamine after oral and smoked administration: a comparative study

      Jordi Riba, Ethan H. McIlhenny, José Carlos Bouso and Steven A. Barker

      Article first published online: 28 JUL 2014 | DOI: 10.1002/dta.1685

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      N,N-dimethyltryptamine, is a natural psychedelic and 5-HT2A agonist of increasing popularity as a recreational drug. Here we report on the metabolism and disposition of DMT when taken by two different routes. Oral intake leads to a lack of psychoactivity due to extensive degradation by monoamine-oxidase. However, smoked intake causes a shift in metabolism from oxidative deamination to less efficient N-oxidation. This shift allows psychoactivity and is analogous to that observed in ayahuasca, a psychotropic preparation combining DMT with MAO inhibitors.

    2. Screening and confirmation of myo-inositol trispyrophosphate (ITPP) in human urine by hydrophilic interaction liquid chromatography high resolution / high accuracy mass spectrometry for doping control purposes

      Christian Görgens, Sven Guddat, Wilhelm Schänzer and Mario Thevis

      Article first published online: 28 JUL 2014 | DOI: 10.1002/dta.1700

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      Myo-inositol trispyrophosphate (ITPP) is a novel allosteric effector of hemoglobin. According to its potential to enhance oxygen release in hypoxic tissues as well as exercising muscles, ITPP is an effective candidate for improving endurance and performance of athletes in sports. According to the molecule's distinct hydrophilic properties, extraction from complex biological matrices is challenging and conventional RPLC separations are not suitable for its detection. Therefore an approach based on hydrophilic interaction liquid chromatography (HILIC) high resolution / high accuracy mass spectrometry was established. To our knowledge, this is the first validated ‘dilute-and-inject’ LC-MS/MS method for the reliable detection of ITPP in human urine without complex sample preparation.

    3. You have free access to this content
      Cannabinoid findings in children hair – what do they really tell us? An assessment in the light of three different analytical methods with focus on interpretation of Δ9-tetrahydrocannabinolic acid A concentrations

      Bjoern Moosmann, Nadine Roth, Martin Hastedt, Andrea Jacobsen-Bauer, Fritz Pragst and Volker Auwärter

      Article first published online: 28 JUL 2014 | DOI: 10.1002/dta.1692

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      We analyzed 79 hair samples of children and their drug-consuming care-givers for THC, THC Acid A, and CBN. Our results suggest that most of the cannabinoids detected in childrens hair usually result from other sources than smoke exposition or active consumption of the child. Furthermore, comparison of three different analytical methods for analysis of cannabinoids in hair revealed that ‘total THC concentrations’ strongly depend on the methodological approach.

    4. Interpretation of group-level factors from a large population dataset in the determination of ethyl glucuronide in hair

      Alberto Salomone, Valentina Pirro, Tonia Lombardo, Daniele Di Corcia, Sergio Pellegrino and Marco Vincenti

      Article first published online: 25 JUL 2014 | DOI: 10.1002/dta.1697

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      Comprehensive results obtained across over 20,000 samples are evaluated to provide a general perspective on HEtG analysis and dependence on group-level factors (e.g., age, gender, site and period of hair collection). The experimental HEtG distributions confirm that chest hair sampling can be trusted as an alternative to scalp. Among biological and external factors, age and season of sampling may significantly influence the HEtG concentration, and this potential source of bias should be taken into account when the results are interpreted.

  7. Short communications

    1. Spatial distribution of theobromine – a low MW drug – in tissues via matrix-free NALDI-MS imaging

      Alessandra Tata, Chiara Montemurro, Andreia M. Porcari, Kamila C. Silva, José B. Lopes de Faria and Marcos N. Eberlin

      Article first published online: 25 JUL 2014 | DOI: 10.1002/dta.1691

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      For the first time, using the accumulation of theobromine drug in rat kidney as a case study,we have successfully demonstrated the ability of nano assisted laser desorption ionization imaging mass spectrometry (NALDI-IMS) to efficiently provide well-resolved spatial distibution of low MW drugs on tissues.

    2. Quantifying cobalt in doping control urine samples – a pilot study

      Oliver Krug, Daniel Kutscher, Thomas Piper, Hans Geyer, Wilhelm Schänzer and Mario Thevis

      Article first published online: 17 JUL 2014 | DOI: 10.1002/dta.1694

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      The possible misuse of cobalt in human and animal sports as an erythropoiesis-stimulating agent is currently under discussion. Therefore, a reference population and doping control samples of endurance athletes were investigated regarding the cobalt content and a preliminary urinary threshold is suggested. Excretion studies performed with a cobalt-containing dietary supplement clearly demonstrated the usefulness of the presented approach.

  8. Correspondence letters

    1. Measurement of iron in serum and EDTA plasma for screening of blood transfusion in sports

      Giuseppe Lippi, Rosalia Aloe, Paola Avanzini and Giuseppe Banfi

      Article first published online: 15 JUL 2014 | DOI: 10.1002/dta.1696

  9. Research articles

    1. Development, optimization, and validation of a novel extraction procedure for the removal of opiates from human hair's surface

      José Restolho, Mário Barroso, Benilde Saramago, Mário Dias and Carlos A.M. Afonso

      Article first published online: 15 JUL 2014 | DOI: 10.1002/dta.1695

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      Contactless opiate extraction from the hair surface relies on the unique properties of ionic liquids (IL). The drugs are irreversibly transported from the hair surface to the bulk of the IL without any physical contact between the phases. The presented method has been found to be more efficient than the conventional methanolic decontamination procedure, and its efficiency is superposable to that of the reference method.

    2. Preparation and characterization of the ‘research chemical’ diphenidine, its pyrrolidine analogue, and their 2,2-diphenylethyl isomers

      Jason Wallach, Pierce V. Kavanagh, Gavin McLaughlin, Noreen Morris, John D. Power, Simon P. Elliott, Marion S. Mercier, David Lodge, Hamilton Morris, Nicola M. Dempster and Simon D. Brandt

      Article first published online: 15 JUL 2014 | DOI: 10.1002/dta.1689

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      Diphenidine has recently appeared as a ‘research chemical’ and belongs to a range of 1,2-diarylethylamines suspected to show dissociative properties. This study presents the synthesis and in-depth characterization of diphenidine, its 2,2-diphenethyl isomer and their pyrrolidine analogues. Analysis of two samples obtained from an Internet vendor provided confirmation that diphenidine was present in both samples. An electrophysiological investigation with rat hippocampal slices also showed that diphenidine reduced N-methyl-D-aspartate (NMDA)-mediated field excitatory postsynaptic potentials similar to ketamine.

    3. Impact of oral fluid collection device on cannabinoid stability following smoked cannabis

      Sébastien Anizan, Mateus M. Bergamaschi, Allan J. Barnes, Garry Milman, Nathalie Desrosiers, Dayong Lee, David A. Gorelick and Marilyn A. Huestis

      Article first published online: 3 JUL 2014 | DOI: 10.1002/dta.1688

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      Cannabinoids stability was evaluated in authentic oral fluid collected with StatSure and Oral-Eze devices. Overall, there were few stability differences between StatSure and Oral-Eze collections. THC and CBD were the most stable analytes collected by each device, and CBN the least. Results suggest performing analyses within 4 weeks of storage at 4 °C for Oral-Eze and within 4 weeks at 4 °C or 24 weeks at −20 °C for StatSure.

  10. Correspondence case reports

  11. Correspondence letters

  12. Research articles

    1. Elucidation of the metabolites of the novel psychoactive substance 4-methyl-N-ethyl-cathinone (4-MEC) in human urine and pooled liver microsomes by GC-MS and LC-HR-MS/MS techniques and of its detectability by GC-MS or LC-MSn standard screening approaches

      Andreas G. Helfer, Alain Turcant, David Boels, Séverine Ferec, Bénédicte Lelièvre, Jessica Welter, Markus R. Meyer and Hans H. Maurer

      Article first published online: 22 JUN 2014 | DOI: 10.1002/dta.1682

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      Studies on the phase I and II metabolism of the novel psychoactive substance 4-methyl-N-ethcathinone (4-MEC)4-MEC in human urine as well as in pooled human liver microsomes are described. 4MEC was metabolized by reduction of the keto group, N-deethylation, hydroxylation followed by oxidation to the corresponding 4-carboxy metabolite, and combinations of these steps. Glucuronidation could be observed for the hydroxy metabolite. An intake of 4-MEC should be detectable in urine by the GC-MS and LC-MSn standard urine screening approaches.

    2. Comparison between drug screening by immunoassay and ultra-high performance liquid chromatography/high-resolution time-of-flight mass spectrometry in post-mortem urine

      Mira Sundström, Anna Pelander and Ilkka Ojanperä

      Article first published online: 20 JUN 2014 | DOI: 10.1002/dta.1683

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      Ultra-high performance liquid chromatography/high resolution time-of-flight mass spectrometry is an attractive technique for comprehensive urine drug screening in terms of scope, sensitivity, and reliability of identification, whereas the widely used immunological tests provide only preliminary results for drugs of abuse while new psychoactive substances often remain undetectable. The performances of these two approaches were critically evaluated. The lower number of false results proved the superiority of the newly developed confirmation-level MS-based method, which has substituted immunoassay in the authors’ laboratory.

    3. Determination of GHB in human hair by HPLC-MS/MS: Development and validation of a method and application to a study group and three possible single exposure cases

      Elisabetta Bertol, Francesco Mari, Fabio Vaiano, Guido Romano, Simona Zaami, Giovanni Baglìo and Francesco Paolo Busardò

      Article first published online: 19 JUN 2014 | DOI: 10.1002/dta.1679

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      This paper develops and fully validates a method for the detection of GHB in human hair by HPLC-MS/MS after liquid-liquid extraction (LLE). The method was applied to hair samples of 30 GHB free-users in order to determine the basal level. A further 12 healthy volunteers, with no previous history of GHB use, were selected and a single dose (25 mg/Kg) was orally administered to all of them and hair samples collected before the administration one month and two months later. This method was applied to three real cases, where a GHB single exposure probably occurred.

    4. Qualitative analysis of seized cocaine samples using desorption electrospray ionization- mass spectrometry (DESI-MS)

      Natasha Stojanovska, Mark Tahtouh, Tamsin Kelly, Alison Beavis and Shanlin Fu

      Article first published online: 17 JUN 2014 | DOI: 10.1002/dta.1684

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      In this study, DESI-MS was utilized in the qualitative analysis of illicit cocaine samples. The effects of a range of adulterants including atropine, paracetamol, procaine, lignocaine, levamisole, and caffeine on the detectability of cocaine were investigated. These adulterants did not prevent the detection of the analyte of interest. DESI-MS was successful in determining the impurities and adulterants present in cocaine samples, indicating the usefulness of the technique.

    5. Metabolic profiling of isomeric aglycones central-icaritin (c-IT) and icaritin (IT) in osteoporotic rats by UPLC-QTOF-MS

      Jun Jiang, Liang Feng, E Sun, Haotian Li, Li Cui and Xiaobin Jia

      Article first published online: 16 JUN 2014 | DOI: 10.1002/dta.1672

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      The anti-osteoporosis effect of c-IT was stronger than IT. According to the metabolites of c-IT and IT revealed by UPLC-Q-TOF-MS, we found that IT could be rapidly conversed to its conjugates after being absorbed, and then be rapidly excreted. However, c-IT had enterohepatic circulation, which further extend its role of anti-osteoporosis efficacy. Finally, c-IT had better therapeutic effect than IT mainly attributed to the less hydroxyl groups in the structure of c-IT compared with IT.

    6. Detection and characterization of emerging psychoactive substances by ion mobility spectrometry

      Sergio Armenta, Salvador Garrigues, Miguel de la Guardia, Judit Brassier, Manel Alcalà, Marcelo Blanco, Clara Perez-Alfonso and Nieves Galipienso

      Article first published online: 16 JUN 2014 | DOI: 10.1002/dta.1678

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      Novel psychoactive substances have been analyzed by ion mobility spectrometry (IMS) and the reduced mobility (K0) values constitute a database to provide a rapid detection and identification of this emerging threat.

    7. Segmental hair analysis for differentiation of tilidine intake from external contamination using LC-ESI-MS/MS and MALDI-MS/MS imaging

      Michael Poetzsch, Markus R. Baumgartner, Andrea E. Steuer and Thomas Kraemer

      Article first published online: 16 JUN 2014 | DOI: 10.1002/dta.1674

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      LC-MS and MALDI-MSI investigations on external tilidine contamination and incorporation into the hair matrix revealed that interpretation of consumption behavior from tilidine hair analysis has to be done with great caution.

  13. Short communications

    1. Rapid assessment of the illegal presence of 1,3-dimethylamylamine (DMAA) in sports nutrition and dietary supplements using 1H NMR spectroscopy

      Yulia B. Monakhova, Maren Ilse, Julia Hengen, Oliver el-Atma, Thomas Kuballa, Matthias Kohl-Himmelseher and Dirk W. Lachenmeier

      Article first published online: 9 JUN 2014 | DOI: 10.1002/dta.1677

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      An NMR spectroscopic method was developed and validated to detect the illegal presence of DMAA in various sports food products and supplements. Nine out of 16 products were found positive (LOD 0.03 g/kg). The method can be recommended for routine use in food testing, customs or doping control laboratories.

  14. Research articles

    1. Doping control analysis of trimetazidine and characterization of major metabolites using mass spectrometric approaches

      Gerd Sigmund, Anja Koch, Anne-Katrin Orlovius, Sven Guddat, Andreas Thomas, Wilhelm Schänzer and Mario Thevis

      Article first published online: 9 JUN 2014 | DOI: 10.1002/dta.1680

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      Using gas chromatography-mass spectrometry and liquid chromatography-high resolution/high accuracy tandem mass spectrometry, trimetazidine and four major metabolites were studied for implementation into routine doping controls. Retrospective data evaluation from 1999 to 2013 demonstrated a substantial prevalence of the anti-anginal drug in elite sport.

    2. Studies on drug metabolism by fungi colonizing decomposing human cadavers. Part II: biotransformation of five model drugs by fungi isolated from post-mortem material

      Jorge A. Martínez-Ramírez, Grit Walther and Frank T. Peters

      Article first published online: 4 JUN 2014 | DOI: 10.1002/dta.1669

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      Five model drugs (MD) were incubated with 28 strains of fungi colonizing cadavers (FCC). The formed metabolites(MB) were identified by liquid chromatography-tandemmass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS). All tested strains were capable of forming mammalian metabolites to a variable extent with some strains additionally producing novel metabolites not previously described in mammals. The results indicate thatFCC may affect drug concentrations and metabolite patterns in post-mortem specimens. The detected novel metabolites are candidates for marker compounds of such changes.

    3. Control of the misuse of testosterone in castrated horses based on an international threshold in plasma

      Emmie N. M. Ho, W. H. Kwok, David K. K. Leung, Christopher M. Riggs, Gordon Sidlow, Brian D. Stewart, April S. Y. Wong and Terence S. M. Wan

      Article first published online: 28 MAY 2014 | DOI: 10.1002/dta.1681

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      The misuse of testosterone in castrated horses has been controlled by an international threshold of free and conjugated testosterone in urine since 1996. In view of the increasing popularity of using blood in doping control testing, it is necessary to establish a threshold for testosterone in gelding plasma. This paper details the establishment of the plasma threshold which provides broadly an equivalent detection time to the international threshold for testosterone in gelding urine.

    4. Comparative study on intestinal metabolism and absorption in vivo of ginsenosides in sulphur-fumigated and non-fumigated ginseng by ultra performance liquid chromatography quadruple time-of-flight mass spectrometry based chemical profiling approach

      He Zhu, Hong Shen, Jun Xu, Jin–Di Xu, Ling–Ying Zhu, Jie Wu, Hu-Biao Chen and Song–Lin Li

      Article first published online: 22 MAY 2014 | DOI: 10.1002/dta.1675

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      Eighteen ginsenoside sulphur derivatives and 26 ginsenoside sulphur derivative metabolites in rat faeces together with 6 ginsenoside sulphur derivatives in rat plasma were identified after oral sulphur-fumigated ginseng, but not identified after oral non-fumigated ginseng, by newly established UHPLC-QTOF-MS/MS analysis. Sulphur-fumigation can significantly affect the intestinal metabolism and absorption of ginseng and should be prohibited before the bioactivity and toxicity of ginsenoside sulphur derivatives were systematically evaluated.

  15. Short communications

    1. A fast automated screening method for the detection of blood transfusion in sports

      Nicolas Leuenberger, Camille Ansermet, Torben Pottgiesser, Norbert Baume, Neil Robinson, Martial Saugy and Yorck Olaf Schumacher

      Article first published online: 22 MAY 2014 | DOI: 10.1002/dta.1676

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      This study showed a strong rise of iron concentration in EDTA-plasma samples after blood transfusion. This method provides excellent supporting information for the Athlete Biological Passport testing to detect autologous and homologous blood transfusion.

  16. Research articles

    1. High-resolution mass spectrometric metabolite profiling of a novel synthetic designer drug, N-(adamantan-1-yl)-1-(5-fluoropentyl)-1H-indole-3-carboxamide (STS-135), using cryopreserved human hepatocytes and assessment of metabolic stability with human liver microsomes

      Adarsh S. Gandhi, Ariane Wohlfarth, Mingshe Zhu, Shaokun Pang, Marisol Castaneto, Karl B. Scheidweiler and Marilyn A. Huestis

      Article first published online: 14 MAY 2014 | DOI: 10.1002/dta.1662

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      More than 25 STS-135 metabolites were identified as oxidized, dealkylated or deflourinated, some of them further glucuronidated. Half-life and intrinsic clearance suggested a highly metabolized drug.

    2. Qualitative analysis of seized synthetic cannabinoids and synthetic cathinones by gas chromatography triple quadrupole tandem mass spectrometry

      Seongshin Gwak, Luis E. Arroyo-Mora and José R. Almirall

      Article first published online: 14 MAY 2014 | DOI: 10.1002/dta.1667

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      This paper describes the identification of 34 designer drugs, mainly synthetic cannabinoids and synthetic cathinones, using gas chromatography-triple quadrupole-tandem mass spectrometry with two different ionization techniques, including electron ionization (EI) and chemical ionization (CI). A larger set of 250 designer drugs has been analyzed by these methods and now compose a commercial database that can be accessed by forensic laboratories for the identification of these drugs, for the first time.

    3. UPLC-MS/MS determination of ephedrine, methylephedrine, amygdalin and glycyrrhizic acid in Beagle plasma and its application to a pharmacokinetic study after oral administration of Ma Huang Tang

      Tianhua Yan, Qiang Fu, Jing Wang and Shiping Ma

      Article first published online: 13 MAY 2014 | DOI: 10.1002/dta.1635

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      In this study, a sensitive and specific LC-ESI-MS/MS method for the quantification of ephedrine, amygdalin and glycyrrhizic acid after oral gavage of MTH in beagle dogs was developed and validated.

    4. In vitro test system for evaluation of immune activation potential of new single-stranded DNA-based therapeutics

      Meltem Avci-Adali, Ludmilla Hann, Tatjana Michel, Heidrun Steinle, Sandra Stoppelkamp, Katharina Stang, Miwako Narita, Christian Schlensak and Hans P. Wendel

      Article first published online: 12 MAY 2014 | DOI: 10.1002/dta.1670

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      A qRT-PCR based assay is established for pre-clinical evaluation of the immune activation potential of newly selected and modified DNA aptamers for in vivo applications. Pooled human whole blood and especially PMDC05 cells show sensitive immune reaction to specific sequences and backbone modifications. Using the established method, preclinical immune activation tests can be performed with new aptamer-based therapeutics.

    5. Evaluation of degradation kinetics and physicochemical stability of tenofovir

      Vivek Agrahari, Sandeep Putty, Christiane Mathes, James B. Murowchick and Bi-Botti C. Youan

      Article first published online: 12 MAY 2014 | DOI: 10.1002/dta.1656

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      This study aimed to investigate the degration behavior and physicochemical stability of Tenofovir (TFV) using a liquid chromatography coupled mass spectrometry and solid state X-ray diffraction analyses. TFV showed degradation under under acidic and alkaline hydrolytic conditions. The structure of degradation products has been proposed. No significant degradation was observed at pH 4.5 (normal CV fluid pH), oxidative, accelerated and thermal stress conditions. The shelf life of TFV at room temperature was found to be 23 months as calculated by using Arrhenius equation plot.

    6. Reliable LC-MS/MS assay for the estimation of rilpivirine in human plasma: application to a bioequivalence study and incurred sample reanalysis

      Ajay Gupta, Swati Guttikar, Yogesh Patel, Pranav S. Shrivastav and Mallika Sanyal

      Article first published online: 9 MAY 2014 | DOI: 10.1002/dta.1665

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      A simple, rugged, and rapid stable isotope dilution liquid chromatography-tandem mass spectrometry method has been developed and validated for the quantification of rilpivirine, a non-nucleoside reverse transcriptase inhibitor in human plasma. The application of the method was demonstrated by a bioequivalence study with 25 mg rilpivirine tablet formulation in 40 healthy subjects. The assay reproducibility was shown by reanalysis of 200 study samples, with % change in the concentration within ±15%.

    7. Metabolites of 5F-AKB-48, a synthetic cannabinoid receptor agonist, identified in human urine and liver microsomal preparations using liquid chromatography high-resolution mass spectrometry

      Niels Bjerre Holm, Anders Just Pedersen, Petur Weihe Dalsgaard and Kristian Linnet

      Article first published online: 6 MAY 2014 | DOI: 10.1002/dta.1663

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      Sixteen phase-I metabolites of 5F-AKB-48 were identified in a human urine sample using LC-HRAM-MS, and compared to the metabolites generated from human liver microsomal incubations. The results may be used in clinical and forensic screening.

    8. Identification and characterization by LC-UV-MS/MS of melanotan II skin-tanning products sold illegally on the Internet

      Torben Breindahl, Michael Evans-Brown, Peter Hindersson, Jim McVeigh, Mark Bellis, Allan Stensballe and Andreas Kimergård

      Article first published online: 25 APR 2014 | DOI: 10.1002/dta.1655

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      New methods were developed and validated to determine the identity, contents, and purity of samples of melanotan II sold illegally as injectable skin-tanning products that were purchased from three online shops. The total amount of melanotan II in vials was different than claimed by the shops and vials from two shops contained unknown impurities. Drugs used for human enhancement purposes are widely available from the illicit market and expose users to potential harms.

    9. Urinary detection of conjugated and unconjugated anabolic steroids by dilute-and-shoot liquid chromatography-high resolution mass spectrometry

      Eva Tudela, Koen Deventer, Lore Geldof and Peter Van Eenoo

      Article first published online: 21 APR 2014 | DOI: 10.1002/dta.1650

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      A validated DS-LC-HRMS method allows to detect 32 conjugated and unconjugated anabolic steroids in urine. The detection limits of 30 of them were in the range 0.5-20 ng mL-1. The application to in vitro experiments and excretion urine permitted the extension of the scope to compounds not commercially available as well as improving knowledge of the metabolism finding better targets compounds. This approach complements more traditional methodologies and sets the stage for future screening methods in doping control.

    10. Copper thiocyanato complexes and cocaine – a case of ‘black cocaine’

      Tim Laussmann, Ireneus Grzesiak, Alexander Krest, Kathrin Stirnat, Sigrid Meier-Giebing, Uwe Ruschewitz and Axel Klein

      Article first published online: 21 APR 2014 | DOI: 10.1002/dta.1658

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      Combined analytical and spectroscopic methods as well as modelling allowed insight into chemical composition, structure, and preparation of a confiscated black powder consisting of cocaine, copper, iron, thiocyanate, and graphite, designed to transport the drug and cloak its detection.

    11. A simple extraction and LC-MS/MS approach for the screening and identification of over 100 analytes in eight different matrices

      Deborah Montenarh, Markus Hopf, Stefan Warth, Hans H. Maurer, Peter Schmidt and Andreas H. Ewald

      Article first published online: 21 APR 2014 | DOI: 10.1002/dta.1657

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      LC-MS/MS multi-analyte method for target screening of benzodiazepines, antidepresssants, neuroleptics, and others in different biosamples after one simple extraction approach is presented. Validation results required for qualitative methods are compared between eight different biosamples.

    12. Evaluation of Δ9-tetrahydrocannabinol detection using DrugWipe5S® screening and oral fluid quantification after Quantisal™ collection for roadside drug detection via a controlled study with chronic cannabis users

      Sarah M. R. Wille, Vincent Di Fazio, Stefan W. Toennes, Janelle H. P. van Wel, Johannes G. Ramaekers and Nele Samyn

      Article first published online: 21 APR 2014 | DOI: 10.1002/dta.1660

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      A double-blind placebo-controlled study (n = 10) was performed. Two subsequent doses of Δ9-tetrahydrocannabinol (THC) were administered using a Volcano vapourizer. Oral fluid (OF) screenings were positive just after smoking; however, sensitivity rapidly decreased within 1.5 h. The collected amount of OF diminished after smoking THC. Chronic cannabis users have high residual THC concentrations in their OF. Confirmation cut-offs should be set according to the aim of detecting recent drug use or establishing zero tolerance when applied to roadside drug testing.

    13. SULT 1A3 single-nucleotide polymorphism and the single dose pharmacokinetics of inhaled salbutamol enantiomers: Are some athletes at risk of higher urine levels?

      Glenn A Jacobson, Kwang Choon Yee, Richard Wood-Baker and E. Haydn Walters

      Article first published online: 1 APR 2014 | DOI: 10.1002/dta.1645

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      Common polymorphisms in the main metabolizing enzyme for salbutamol (SULTA1A3; 105A>G sSNP (rs1975350) do not put some athletes at risk of higher urine levels and adverse analytical findings.

    14. Targeting misuse of 2-amino-N-ethyl-1-phenylbutane in urine samples: in vitro–in vivo correlation of metabolic profiles and development of LC-TOF-MS method

      Masaki Kobayashi, Anna Pelander, Raimo A. Ketola, Antti Leinonen and Tiia Kuuranne

      Article first published online: 28 MAR 2014 | DOI: 10.1002/dta.1642

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      Routine mass spectrometric detection methods targeted to amphetamine derivatives can be easily extended to monitor a phenyethylamine derivative, 2-amino-N-ethyl-1-phenylbutane (2-AEPB), in doping control and drugs-of-abuse analysis of urine samples.

    15. HILIC-UPLC-MS/MS combined with hierarchical clustering analysis to rapidly analyze and evaluate nucleobases and nucleosides in Ginkgo biloba leaves

      Xin Yao, Guisheng Zhou, Yuping Tang, Sheng Guo, Dawei Qian and Jin-ao Duan

      Article first published online: 24 MAR 2014 | DOI: 10.1002/dta.1634

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      A HILIC-UPLC-TQ-MS/MS has been successfully developed and employed to determine 11 nucleosides and nucleobases in G. biloba leaves. The established approach could be helpful for evaluation of the potential values as dietary supplements and the quality control of G. biloba leaves, which might also be utilized for the investigation of other medicinal herbs containing nucleobases and nucleosides.

    16. Production of human metabolites by gastrointestinal bacteria as a potential source of post-mortem alteration of antemortem drug/metabolite concentrations

      Stephanie M. Martindale, Robert H. Powers and Suzanne C. Bell

      Article first published online: 24 MAR 2014 | DOI: 10.1002/dta.1647

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      This research investigated the effects of Escherichia coli, Bacteroides fragilis, and Clostridium perfringens on drugs of abuse and compared bacterial biotransformation products to those of human metabolism. Diazepam samples inoculated with Escherichia coli and Bacteroides fragilis demonstrated a decrease in concentration between pre- and post-incubation; however there was no corresponding increase in concentration for the monitored human metabolites. Bacteroides fragilis, Clostridium perfringens, and mixed culture resulted in nearly complete conversion of flunitrazepam to 7-aminoflunitrazepam.

  17. Correspondence case reports

    1. What's the deal? Trends in Irish street-level heroin and cocaine 2010-2012

      Michelle Boyle, Lynn Carroll, Karen Clarke, Paula Clarke, Hugh J. Coyle, Henry English, Miriam Goff, Eugene Kane, Sarah Killoran and Kristen O'Connor

      Article first published online: 24 MAR 2014 | DOI: 10.1002/dta.1639

  18. Research articles

    1. Cannabinoid disposition in oral fluid after controlled cannabis smoking in frequent and occasional smokers

      Matthew N. Newmeyer, Nathalie A. Desrosiers, Dayong Lee, Damodara R. Mendu, Allan J. Barnes, David A. Gorelick and Marilyn A. Huestis

      Article first published online: 20 MAR 2014 | DOI: 10.1002/dta.1632

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      Quantification of multiple oral fluid (OF) cannabinoids improves test interpretation, but differences in OF cannabinoid pharmacokinetics between frequent and occasional smokers are not fully characterized. Additionally, it is unclear if the new Oral-Eze® OF collection device will perform similarly to other commercially available devices. Our data illustrate the effectiveness of the Oral-Eze® device for OF collection, the impact of self-administered smoked cannabis history on OF cannabinoid results, and the ability to improve interpretation and tailor OF cannabinoid cut-offs to fulfill the detection window needs of different drug testing programs.

  19. Perspectives

    1. Workplace drug testing in Italy: Findings about second-stage testing

      Claudia Vignali, Cristiana Stramesi, Luca Morini, Paolo San Bartolomeo and Angelo Groppi

      Article first published online: 20 MAR 2014 | DOI: 10.1002/dta.1640

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      We analyzed urine and hair specimens from 120 workers undergoing second-level testing between 2009 and 2012. As regards urine samples, 71.2% of workers were always negative, 23.9% tested positive at least once for cannabinoids, and 2.5% for cocaine. Hair analyses produced surprising results: 61.9% of hair samples tested negative, only 6.2% tested positive for cannabinoids, whereas 28.8% tested positive for cocaine. These findings confirm that second-level surveillance of WDT, which includes hair analysis, is very effective because it highlightd drug intake – sometimes heavy – that cannot be revealed through a few urine analyses.

  20. Research articles

    1. Metabolic pathways of anthelmintic drug monepantel in sheep and in its parasite (Haemonchus contortus)

      Lucie Stuchlíková, Robert Jirásko, Ivan Vokřál, Martin Valát, Jiří Lamka, Barbora Szotáková, Michal Holčapek and Lenka Skálová

      Article first published online: 10 MAR 2014 | DOI: 10.1002/dta.1630

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      Biotransformation of monepantel (MOP) was studied in sheep in vivo and in its parasite Haemonchus contortus ex vivo. UHPLC-MS/MS analysis led to the identification of 13 MOP metabolites in ovine urine, faeces and 4 MOP metabolites in nematodes. Based on obtained results, schemes of metabolic pathways of MOP in sheep and nematodes were proposed.

    2. Lefetamine-derived designer drugs N-ethyl-1,2-diphenylethylamine (NEDPA) and N-iso-propyl-1,2-diphenylethylamine (NPDPA): Metabolism and detectability in rat urine using GC-MS, LC-MSn and LC-HR-MS/MS

      Carina S. D. Wink, Golo M. J. Meyer, Dirk K. Wissenbach, Andrea Jacobsen-Bauer, Markus R. Meyer and Hans H. Maurer

      Article first published online: 3 MAR 2014 | DOI: 10.1002/dta.1621

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      N-Ethyl-1,2-diphenylethylamine (NEDPA) and N-iso-propyl-1,2-diphenylethylamine (NPDPA) are two new designer drugs, derived from the scheduled drug lefetamine. The present work describes phase I and phase II metabolism of these drugs in rat urine studied using GC-MS and LC-HR-MS/MS and the detectability of an intake in urine using the authors’ GC-MS and LC-MSn standard urine.

    3. A high-throughput LC-MS/MS screen for GHRP in equine and human urine, featuring peptide derivatization for improved chromatography

      Mark Timms, Nikki Hall, Vita Levina, John Vine and Rohan Steel

      Article first published online: 24 FEB 2014 | DOI: 10.1002/dta.1624

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      A method for extracting, derivatising and detecting GHRP in equine and human urine by LC/MS/MS. Derivatisation is used to neutralise basic amino acid residues, improving reversed phase chromatography in difficult matrices.

    4. Factors influencing total carbon dioxide concentrations in plasma of thoroughbred and standardbred racehorses

      Gordon J. Sutton, Adam Cawley, Cary Murphy, Marcus L. Lau and D. Brynn Hibbert

      Article first published online: 24 FEB 2014 | DOI: 10.1002/dta.1600

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      The similarities and differences between the distributions of ‘total carbon dioxide’ concentrations in plasma of thoroughbred (flat racing, gallops) and standardbred (harness racing, trotters) racehorses are explored. Seasonal variations in the distribution means were identified and found similar for the two populations, with the effects peaking in winter. Evidence of a small standardbred subpopulation with a raised mean was found, suggesting some degree of alkalinising salts were being administered.

    5. Determination of levamisole, aminorex, and pemoline in plasma by means of liquid chromatography-mass spectrometry and application to a pharmacokinetic study of levamisole

      Cornelius Hess, Natalie Ritke, Konrad Sydow, Lena-Maria Mehling, Hauke Ruehs, Burkhard Madea and Frank Musshoff

      Article first published online: 20 FEB 2014 | DOI: 10.1002/dta.1619

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      Aminorex was found to be a metabolite of levamisole. It could be determined in plasma and urine samples after administration of levamisole or after misuse of cocaine, however, in very low concentrations. Pemoline, an oxidation product of aminorex found in equine urine, could not be detected in human material.

    6. Drug-drug interaction and doping, part 2: An in vitro study on the effect of non-prohibited drugs on the phase I metabolic profile of stanozolol

      Monica Mazzarino, Xavier de la Torre, Ilaria Fiacco and Francesco Botrè

      Article first published online: 17 FEB 2014 | DOI: 10.1002/dta.1608

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      This study was designed to provide information on the effects that drug-drug interaction might have on the effectiveness of the strategies currently followed by anti-doping laboratories to detect the intake of banned agents. In vitro assays were applied to characterize the metabolic profile of the synthetic anabolic androgenic steroid stanozolol in the absence and in the presence of medicaments commonly administered to athletes. The results show that antifungals and antidepressants caused significant alteration of the stanozolol metabolic profile.

    7. Direct analysis of traditional Chinese medicines using surface-enhanced raman scattering (SERS)

      Jing Zhao, Yang Liu, Andrew M. Fales, Janna Register, Hsiangkuo Yuan and Tuan Vo-Dinh

      Article first published online: 12 FEB 2014 | DOI: 10.1002/dta.1612

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      The potential of SERS was demonstrated as a sensitive, rapid, and non-destructive method to qualitatively and quantitatively analyze the active constituents in raw TCM products. Two important TCMs, namely Coptis chinensis and Phellodendron amurense, and their main active constituent, berberine were analyzed. The results were consistent with the results of DFT calculations and LCMS analyses.

    8. Prospective evaluation of potential toxicity of repeated doses of Thymus vulgaris L. extracts in rats by means of clinical chemistry, histopathology and NMR-based metabonomic approach

      Fouzia Benourad, Zehra Kahvecioglu, Mokhtar Youcef-Benkada and Jean-Marie Colet

      Article first published online: 12 FEB 2014 | DOI: 10.1002/dta.1606

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      Compared with the negative results of the histopathology examinations of the liver and kidney tissues, the metabonomics study did highlight some slight variations in the urine excretion of some metabolites.

    9. Studies on the minor metabolite 6a-hydroxy-androstenedione for doping control purposes and its contribution to the steroid profile

      Michael Polet, Pieter Van Renterghem, Wim Van Gansbeke and Peter Van Eenoo

      Article first published online: 11 FEB 2014 | DOI: 10.1002/dta.1618

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      This study encompasses 6aOH-ADION reference population data (n = 2128) measured with GCMS/MS. A urinary concentration threshold of 5 ng/mL was set. Concentrations above this threshold are considered as suspicious and are forwarded to IRMS for confirmation in routine practice.

    10. Docetaxel epimerization in silicone films: a case of drug excipient incompatibility

      Shaikh Mohsin, Ian Harvey Arellano, Namita Roy Choudhury and Sanjay Garg

      Article first published online: 11 FEB 2014 | DOI: 10.1002/dta.1617

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      An atypical case of Docetaxel (DTX) epimerization within the drug-eluting silicone films is facilitated mainly by the tin catalyst, a usual component of room temperature curing silicone products, and partly by the release media.

    11. Variability of blood alcohol content (BAC) determinations: The role of measurement uncertainty, significant figures, and decision rules for compliance assessment in the frame of a multiple BAC threshold law

      Luca Zamengo, Giampietro Frison, Gianpaola Tedeschi, Samuela Frasson, Flavio Zancanaro and Rocco Sciarrone

      Article first published online: 30 JAN 2014 | DOI: 10.1002/dta.1614

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      The aims of this study were: (1) to investigate major sources of variability for BAC determinations; (2) to estimate measurement uncertainty for routine BAC determinations; (3) to discuss the role of measurement uncertainty in compliance assessment; (4) to set decision rules for a multi-level BAC threshold law, as provided in the Italian road traffic legislation; (5) to address the topic of the zero-alcohol limit from the forensic toxicology point of view; and (6) to discuss the role of significant figures and rounding errors on measurement accuracy and compliance assessment.

    12. Development and comparison of two competitive ELISAs for estimation of cotinine in human exposed to environmental tobacco smoke

      Yajing Lei, Qian Zhang, Lizheng Fang, Muhammad Sajid Hamid Akash, Kanwal Rehman, Zhiming Liu, Weixing Shi and Shuqing Chen

      Article first published online: 27 JAN 2014 | DOI: 10.1002/dta.1609

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      Cotinine is a biomarker for the estimation of ETS in population but its detection is rather difficult and complicated. We developed a direct competitive ELISA for the estimation of COT from urine samples and compared it with indirect competitive ELISA. The comparative results of the two competitive ELISAs (direct vs. indirect) indicate that our developed method is simple, precise, and can be applied for the routine analysis and high throughput determination of COT in urine.

    13. Assessment of different mouthwashes on cannabis oral fluid concentrations

      Ana de Castro, Elena Lendoiro, Hadriana Fernández-Vega, Manuel López-Rivadulla, Stefan Steinmeyer and Angelines Cruz

      Article first published online: 22 JAN 2014 | DOI: 10.1002/dta.1605

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      We evaluate the effect of different mouthwashes on tetrahydrocannabinol (THC) oral fluid concentrations, and those observed in passive smokers subjected to extreme contamination conditions. THC concentrations at t= 0.25h were >3-fold higher than the cut-off employed by the Spanish police (25 ng/mL) regardless of the use of any mouthwash. THC was found in passive smokers' oral fluid, although at concentrations <25 ng/mL.

    14. Fatty acid ethyl esters in hair: correlation with self-reported ethanol intake in 160 subjects and influence of estroprogestin therapy

      Elisabetta Bertol, Ester Del Bravo, Fabio Vaiano, Francesco Mari and Donata Favretto

      Article first published online: 15 JAN 2014 | DOI: 10.1002/dta.1595

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      Fatty acid ethyl esters are minor ethanol metabolites that can accumulate in hair. To verify their performance as a biomarker discriminating null or moderate drinking from risky drinking, the relationship between selfreported daily alcohol intake and fatty acid ethyl esters in hair was studied in 160 healthy volunteers including teetotalers, moderate and social drinkers (< 60 g of ethanol per day) and heavy drinkers (≥ 60 g/day).

    15. PPARgamma agonist pioglitazone does not enhance performance in mice

      Fabian Sanchis-Gomar, Helios Pareja-Galeano and Vladimir E. Martinez-Bello

      Article first published online: 20 NOV 2013 | DOI: 10.1002/dta.1587

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      To date, experimental evidence revealed that PPARgamma agonist could induce the same biological effects in glucose metabolism, mitochondrial biogenesis, skeletal muscle fiber type, and physical performance as the prohibited drug GW1516 and AICAR, modulators of PPARdelta and AMPK respectively. However, as we describe in the present article, treatment with PPARgamma agonist pioglitazone does not regulate the glucose profile nor mitochondrial biogenesis machinery in soleus and gastrocnemius. In addition, pioglitazone does not improve physical performance measured by maximal aerobic velocity, endurance capacity and grip strength in mice.

    16. A high throughput screen for 17 Dermorphin peptides in equine and human urine and equine plasma

      Rohan Steel, Mark Timms, Vita Levina and John Vine

      Article first published online: 20 NOV 2013 | DOI: 10.1002/dta.1585

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      A high throughput LC-MS/MS screen using a novel mixed-mode SPE method to detect 17 Dermorphin peptides in equine urine and plasma with limits of detection down to 5 pg/mL.

    17. Experimental design for the optimization and robustness testing of a liquid chromatography tandem mass spectrometry method for the trace analysis of the potentially genotoxic 1,3-diisopropylurea

      György Székely, Bruno Henriques, Marco Gil and Carlos Alvarez

      Article first published online: 15 NOV 2013 | DOI: 10.1002/dta.1583

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      It is demonstrated that the DoE approach exploring both LC and MS parameters together – rather than in the conventional consecutive manner – reveals unpredictable method development obstacles at an early stage, and thus rapidly leads to more accurate methods. The novel LC-MS/MS method meets criteria such as ease of use, low cost per analysis, ultra-low LOQ, high sample throughput, and robustness.

    18. Workplace drug testing and alcohol policy in Italy; there is still a long way to go

      Gian Luca Rosso, Massimo Perotto, Mauro Feola and Michele Caramella

      Article first published online: 25 OCT 2013 | DOI: 10.1002/dta.1569

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      Workplace drug testing (WDT) effectiveness and alcoholic beverage consumption among Italian professional drivers (PDs) have been investigated. In our sample, only 30% of Italian PDs were correctly subjected to WDT with a real surprise effect. We describe the main factors associated with alcohol consumption during working hours. Fifteen percent of PDs seem to be hazardous drinkers.

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