Drug Testing and Analysis

Cover image for Vol. 9 Issue 7

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

Editor-in-Chief: Prof. Mario Thevis

Impact Factor: 3.469

ISI Journal Citation Reports © Ranking: 2016: 15/76 (Chemistry Analytical); 25/77 (BIOCHEMICAL RESEARCH METHODS); 62/256 (Pharmacology & Pharmacy)

Online ISSN: 1942-7611

VIEW

  1. 1 - 78
  1. RESEARCH ARTICLES

    1. Fatal intoxication by 5F–ADB and diphenidine: Detection, quantification, and investigation of their main metabolic pathways in humans by LC/MS/MS and LC/Q-TOFMS

      Maiko Kusano, Kei Zaitsu, Kentaro Taki, Kazuaki Hisatsune, Jun'ichi Nakajima, Takako Moriyasu, Tomomi Asano, Yumi Hayashi, Hitoshi Tsuchihashi and Akira Ishii

      Version of Record online: 19 JUL 2017 | DOI: 10.1002/dta.2215

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      We describe the detection and quantification of new psychoactive substances 5F–ADB and diphenidine in an acute intoxication case using LC/MS/MS and LC/Q-TOFMS. This is the first report of postmortem blood concentration and the metabolic pathway of 5F–ADB in humans.

  2. SHORT COMMUNICATIONS

    1. Identification and quantification of predominant metabolites of synthetic cannabinoid MAB-CHMINACA in an authentic human urine specimen

      Koutaro Hasegawa, Kayoko Minakata, Kunio Gonmori, Hideki Nozawa, Itaru Yamagishi, Kanako Watanabe and Osamu Suzuki

      Version of Record online: 19 JUL 2017 | DOI: 10.1002/dta.2220

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      The MAB-CHMINACA metabolites from the urine specimen of an abuser were extracted by a QuEChERS method, and analyzed by liquid chromatography-tandem mass spectrometry. Among the six MAB-CHMINACA metabolites tested, 2 predominant metabolites (monohydroxyl metabolite M1 and dihydroxyl metabolite M11) could be identified and quantified (2.17±0.15 and 10.2±0.3 ng/mL for M1 and M11, respectively). This is the first report dealing with in vivo identification and quantification of MAB-CHMINACA metabolites in an authentic human urine specimen.

  3. RESEARCH ARTICLES

    1. Ultra-fast LC–MS/MS in therapeutic drug monitoring: Quantification of clozapine and norclozapine in human plasma

      Lewis Couchman, Danielle S. Fisher, Krithika Subramaniam, Simon A. Handley, Robert J. Boughtflower, Christopher M. Benton and Robert J. Flanagan

      Version of Record online: 19 JUL 2017 | DOI: 10.1002/dta.2223

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      A novel approach to ultra-rapid, high-throughput LC–MS/MS analysis has been developed. The total analysis time was just 36 s per injection, or one 96-well plate of prepared samples per hour, for the demonstrated application of clozapine and norclozapine analysis in human plasma samples. This approach is simple, and is likely to be ideally suited to a number of targeted assays.

    2. Replacing PAPS: In vitro phase II sulfation of steroids with the liver S9 fraction employing ATP and sodium sulfate

      Sumudu A. Weththasinghe, Christopher C. Waller, Han Ling Fam, Bradley J. Stevenson, Adam T. Cawley and Malcolm D. McLeod

      Version of Record online: 18 JUL 2017 | DOI: 10.1002/dta.2224

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      Replacing the expensive and unstable PAPS cofactor with ATP and sodium sulfate provides a cost-effective alternative to study in vitro phase II sulfation using the liver S9 fraction. The scope of this approach is demonstrated for the human, equine, and canine sulfation of six representative steroids. The in vitro metabolism of the designer steroids furazadrol and superdrol is also reported.

    3. The effect of antioxidants on the long-term stability of THC and related cannabinoids in sampled whole blood

      Lambert K. Sørensen and Jørgen B. Hasselstrøm

      Version of Record online: 18 JUL 2017 | DOI: 10.1002/dta.2221

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      THC and related cannabinoids were instable in whole blood stored at −20°C, especially when interrupted by several thawing/freezing cycles. The measured concentrations of THC and CBD in authentic field samples of whole blood preserved solely with fluoride citrate or fluoride oxalate mixtures decreased on average to less than 5% of the initial concentrations after 19 weeks of storage interrupted by 5 thawing/freezing cycles. The instability was avoided by adding 30 mM ascorbic acid (ASC) to the blood samples before storage.

  4. SHORT COMMUNICATIONS

    1. Drug residues in syringes and other injecting paraphernalia in Hungary

      Anna Péterfi, József Csorba, Tamás Figeczki, József Kiss, Katalin Medgyesi-Frank, János Posta and V. Anna Gyarmathy

      Version of Record online: 18 JUL 2017 | DOI: 10.1002/dta.2217

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      The injection of synthetic cathinones as the main pattern among Hungarian people who inject drugs and the large-scale diversion and abuse of methadone are the main results of the study. The findings are based on the chemical analysis of used and discarded injecting paraphernalia collected throughout a 12-month period involving seven study locations in Hungary.

    2. Analytical characterization of three cathinone derivatives, 4-MPD, 4F–PHP and bk-EPDP, purchased as bulk powder from online vendors

      Orapan Apirakkan, Anca Frinculescu, Trevor Shine, Mark C. Parkin, Agostino Cilibrizzi, Nunzianda Frascione and Vincenzo Abbate

      Version of Record online: 18 JUL 2017 | DOI: 10.1002/dta.2218

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      This paper describes the detection, identification and full structural elucidation of three emerging cathinone derivatives, 4-MPD, 4F–PHP and bk-EPDP, purchased as bulk powders online from ‘legal high’ websites.

  5. ERRATA

    1. You have free access to this content
  6. RESEARCH ARTICLES

    1. Chiral analysis of amphetamines in hair by liquid chromatography–tandem mass spectrometry: compliance-monitoring of attention deficit hyperactivity disorder (ADHD) patients under Elvanse® therapy and identification after controlled low-dose application

      Tina M. Binz, Elena Williner, Petra Strajhar, Patrick C. Dolder, Matthias E. Liechti, Markus R. Baumgartner, Thomas Kraemer and Andrea E. Steuer

      Version of Record online: 5 JUL 2017 | DOI: 10.1002/dta.2208

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      This study describes the successful development and validation of an LC–MS/MS method for the qualitative and quantitative analysis of (S)-amphetamine and (R)-amphetamine in hair. With this method it is now possible to differentiate between the intake of medically prescribed (S)-amphetamine and illegal street amphetamine by the use of hair analysis. Furthermore, it could be shown that after a low oral dose of lisdexamfetamine, (S)-amphetamine can still be detected in hair which can be of great importance in forensic toxicology.

  7. SHORT COMMUNICATIONS

    1. Ephedra alkaloid contents of Chinese herbal formulae sold in Taiwan

      Chih-Wei Chang, Szu-Yun Hsu, Guan-Qian Huang and Mei-Chich Hsu

      Version of Record online: 23 JUN 2017 | DOI: 10.1002/dta.2209

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      This is the first study to systematically determine the Ephedra alkaloid contents of the Chinese herbal formula products sold in Taiwan. Using their E/PE and E/total ratios, we identified that the Herba Ephedrae species used in the products was probably E. sinica or E. equisetina, but not E. intermedia. Among the 56 tested samples, we discovered that a single dose of half of them would probably result in a threshold violation.

  8. Research articles

    1. Influence of bleaching and coloring on ethyl glucuronide content in human hair

      Silvana Petzel-Witt, Werner Pogoda, Cora Wunder, Alexander Paulke, Manfred Schubert-Zsilavecz and Stefan W. Toennes

      Version of Record online: 22 JUN 2017 | DOI: 10.1002/dta.2206

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      Different hair colouring procedures were performed with 12 EtG positive hair samples, including treatment with henna. The expected marked reductions in EtG contents even below the LOD were found. Unexpectedly, treatment with henna also affected EtG content massively.

    2. Interlaboratory trial for the measurement of total cobalt in equine urine and plasma by ICP-MS

      Marie-Agnes Popot, Emmie N.M. Ho, Natali Stojiljkovic, Florian Bagilet, Pierre Remy, Pascal Maciejewski, Benoit Loup, George H.M. Chan, Sabine Hargrave, Rick M. Arthur, Charlie Russo, James White, Pamela Hincks, Clive Pearce, George Ganio, Paul Zahra, David Batty, Mark Jarrett, Lydia Brooks, Lise-Anne Prescott, Ludovic Bailly-Chouriberry, Yves Bonnaire and Terence S.M. Wan

      Version of Record online: 20 JUN 2017 | DOI: 10.1002/dta.2191

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      In order to control the misuse of cobalt, It was necessary to establish an international threshold for cobalt in plasma and/or in urine. An international collaboration, consisting of an interlaboratory comparison, between 5 laboratories for the urine study and 8 laboratories for plasma study has been successfully undertaken.

    3. Identification, isolation, and synthesis of seven novel impurities of anti-diabetic drug Repaglinide

      Prasad Kancherla, Srinivas Keesari, Pallavi Alegete, Mukkanti Khagga and Parthasarathi Das

      Version of Record online: 20 JUN 2017 | DOI: 10.1002/dta.2207

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      Seven unknown impurities in repaglinide 1 bulk drug batches at below 0.1 level were detected by an ultra performance liquid chromatographic (UPLC) method. The spectral analysis e.g. 1H NMR, 13C NMR, MS and IR confirmed the proposed chemical structures of impurities. Identification, complete characterization data and their synthesis were reported for the first time.

  9. SHORT COMMUNICATIONS

    1. Analysis of RBC-microparticles in stored whole blood bags – a promising marker to detect blood doping in sports?

      Sven Christian Voss, Morana Jaganjac, Amna Mohamed Al-Thani, Jean-Charles Grivel, Christophe Michel Raynaud, Hind Al-Jaber, Afnan Saleh Al-Menhali, Zeyed Ahmad Merenkov, Mohammed Alsayrafi, Aishah Latiff and Costas Georgakopoulos

      Version of Record online: 20 JUN 2017 | DOI: 10.1002/dta.2212

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      The goal of this study was to investigate red blood cell microparticles (RBC-MPs) during storage in CPDA-1 blood bags. Blood was analyzed on day 0 and after 14 and 35 days of storage using the new Apogee Flow Systems A-60 Micro-Plus flow cytometer. The number of RBC-MPs increased significantly during the study (approx. 100-fold). RBC-MPs have the potential as possible a biomarker for the detection of autologous blood transfusion.

  10. Research articles

    1. Two complementary methods to control gonadotropin-releasing hormone vaccination (Improvac®) misuse in horseracing: Enzyme-linked immunosorbent assay test in plasma and steroidomics in urine

      Ludovic Bailly-Chouriberry, Benoit Loup, Marie-Agnès Popot, Marie-Laure Dreau, Patrice Garcia, Jean-François Bruyas and Yves Bonnaire

      Version of Record online: 2 JUN 2017 | DOI: 10.1002/dta.2187

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      Two new analytical approaches are proposed to the horseracing industry to prevent Improvac® misuse. These are an enzyme-linked immunosorbent assay test to detect anti-gonadotropin-releasing hormone antibodies in plasma and a complementary study with urine by steroidomics. The two methods allow the control of immunological castration.

    2. Evidence of boldenone, nandrolone, 5(10)-estrene-3β-17α-diol and 4-estrene-3,17-dione as minor metabolites of testosterone in equine

      Jenny K. Y. Wong, David K. K. Leung, Peter Curl, Peter J. Schiff, Kenneth K. H. Lam and Terence S. M. Wan

      Version of Record online: 1 JUN 2017 | DOI: 10.1002/dta.2192

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      Low levels of boldenone, nandrolone, 5(10)-estrene-3β,17α-diol, and 4-estrene-3,17-dione could detected and confirmed in the early post-administration urine samples in six gelding horses administered with ‘Testosterone Suspension 100’. A tracer experiment was carried out by administering a 1:1 mixture of 13C–testosterone and Testosterone Suspension 100. Indeed, 13C–labelled boldenone, 4-estrene-3-17-dione and nandrolone were detected in post-administration urine and provide the first unequivocal evidence that these steroids are metabolites of testosterone in geldings.

    3. RNA sample preparation applied to gene expression profiling for the horse biological passport

      Ludovic Bailly-Chouriberry, Florent Baudoin, Florence Cormant, Yohan Glavieux, Benoit Loup, Patrice Garcia, Marie-Agnès Popot and Yves Bonnaire

      Version of Record online: 31 MAY 2017 | DOI: 10.1002/dta.2204

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      The present study described the possibility to use a modified version of the dedicated human IVD PAXgene® Blood RNA Kit for gene expression analysis from horse blood collected on PAXgene® tubes applied to the horse biological passport.

  11. Short communications

    1. Identification of pyrolysis products of the new psychoactive substance 2-amino-1-(4-bromo-2,5-dimethoxyphenyl)ethanone hydrochloride (bk-2C-B) and its iodo analogue bk-2C-I

      Kelly B. Texter, Rachel Waymach, Pierce V. Kavanagh, John E. O'Brien, Brian Talbot, Simon D. Brandt and Elizabeth A. Gardner

      Version of Record online: 31 MAY 2017 | DOI: 10.1002/dta.2200

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      A study of the pyrolysis of two new beta keto analog of 2-(4-bromo-2,5-dimethoxyphenyl) ethan-1-amine (2C–B), bk-2C-1. Products were formed by deamination, loss of the bk oxygen and halogenation.

  12. Research articles

    1. lmplementation of the prolyl hydroxylase inhibitor Roxadustat (FG-4592) and its main metabolites into routine doping controls

      Daniel Eichner, Ryan M. Van Wagoner, Mitch Brenner, James Chou, Scott Leigh, Lee R. Wright, Lee A. Flippin, Michael Martinelli, Oliver Krug, Wilhelm Schänzer and Mario Thevis

      Version of Record online: 31 MAY 2017 | DOI: 10.1002/dta.2202

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      Updating and expanding routine doping control assays is vital for efficient sports drug testing programs. HIF stabilizers have been identified as a new class of substances being misused in sports, and the comprehensive analysis of FG-4592 (Roxadustat) inclusive of its main metabolites and a light-induced rearrangement artifact is presented.

    2. Doping control study of AICAR in post-race urine and plasma samples from horses

      Jenny K. Y. Wong, Wai Him Kwok, George H. M. Chan, Timmy L. S. Choi, Emmie N. M. Ho, Murielle Jaubert, Ludovic Bailly-Chouriberry, Yves Bonnaire, Adam Cawley, H. Ming Williams, John Keledjian, Lydia Brooks, Adam Chambers, Yuanyuan Lin and Terence S. M. Wan

      Version of Record online: 31 MAY 2017 | DOI: 10.1002/dta.2205

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      AICAR is an endogenous AMPK activator in many mammals, including horses. It has attracted considerable attention in the field of doping control because of its potential endurance enhancing effect. This paper presents the statistical evaluation of AICAR in horse urine using population data acquired in three countries. A urinary screening cut-off at 600 ng/mL could be considered for adoption for the control of excessive AICAR in equine urine.

  13. Special feature: reviews

    1. Equine performance genes and the future of doping in horseracing

      Tessa Wilkin, Anna Baoutina and Natasha Hamilton

      Version of Record online: 30 MAY 2017 | DOI: 10.1002/dta.2198

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      Gene doping is predicted to be the next phase of doping faced by horseracing. Development of an equine gene doping test will first require identification of equine genes that will likely be targeted by gene doping attempts. This review focuses on genes that have been linked to athletic performance in horses and, therefore, could be targeted for genetic manipulation.

  14. Research articles

    1. Detection of the recently emerged synthetic cannabinoid 5F–MDMB-PICA in ‘legal high’ products and human urine samples

      Lukas Mogler, Florian Franz, Daniel Rentsch, Verena Angerer, Georg Weinfurtner, Mitchell Longworth, Samuel D. Banister, Michael Kassiou, Bjoern Moosmann and Volker Auwärter

      Version of Record online: 24 MAY 2017 | DOI: 10.1002/dta.2201

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      Signals for metabolites of the SC 5F-PB-22 during routine LC-MS/MS screening of urine specimens for SC metabolites were identified as metabolites of the novel synthetic cannabinoid SC 5F-MDMB-PICA by LC-QToF-MS analysis. In this study the detection 5F-MDMB-PICA in herbal blends adn the identification of phase I metabolites suitable for proving 5F-MDMB-PICA consumption by LC-MS/MS and LC-Q-ToF-MS analyses of authentic urine samples is reported. Commercial available immunochemical pre-tests were tested for the detection of 5F-MDMB-PICA consumption.

    2. Report on an anti-doping operation in Guadeloupe: High number of positive cases and inferences about doping habits

      A. Marchand, C. Buisson, L. Martin, J.-A. Martin, A. Molina and D. Ressiot

      Version of Record online: 24 MAY 2017 | DOI: 10.1002/dta.2185

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      The results of an anti-doping operation performed during a regional cycling race in Guadeloupe in March 2016 are presented. Serum and urine samples from 42 athletes were analysed. Four CERA, one rEPO and one GH were identified in serum samples. Stimulants heptaminol and DMBA and glucocorticoids prednisone/prednisolone were also found in some urines. Altogether, 7 of 42 athletes tested (16.6%) were reported with adverse analytical findings. Interestingly, CERA and rEPO were not retrieved in urine, and would have been missed without serum analyses.

    3. Flubromazolam – Basic pharmacokinetic evaluation of a highly potent designer benzodiazepine

      Laura M. Huppertz, Bjoern Moosmann and Volker Auwärter

      Version of Record online: 19 MAY 2017 | DOI: 10.1002/dta.2203

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      Designer benzodiazepines are a quickly growing class of compounds among new psychoactive substances. We report on the period of detectability in biological samples and present basic pharmacokinetic data of the highly potent, rather long-acting designer benzodiazepine flubromazolam, a compound which might well be used in drug facilitated crimes.

    4. Oral absorption, distribution, metabolism, and excretion of icaritin in rats by Q-TOF and UHPLC–MS/MS

      Shuang-Qing Zhang and Shi-Zhong Zhang

      Version of Record online: 15 MAY 2017 | DOI: 10.1002/dta.2188

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      Absorption, distribution, metabolism, and excretion of ICT were first investigated. Metabolites of ICT were first identified by Q-TOF.

  15. Short communications

    1. Determination of cannabinoid and synthetic cannabinoid metabolites in wastewater by liquid–liquid extraction and ultra-high performance supercritical fluid chromatography-tandem mass spectrometry

      Iria González-Mariño, Kevin V. Thomas and Malcolm J. Reid

      Version of Record online: 12 MAY 2017 | DOI: 10.1002/dta.2199

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      Ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry is used to determine cannabinoid and synthetic cannabinoid residues in wastewater. Combined with a simple liquid-liquid extraction procedure, it provides a rapid and simple method for the quantification of Δ9-tetrahydrocannabinol, three of its major metabolites (the monohydroxylated, the dihydroxylated and the carboxylated species) and four synthetic cannabinoid metabolites (from the JWH-series) at low ng L-1 levels.

  16. Research articles

    1. Identification and characterization of novel long-term metabolites of oxymesterone and mesterolone in human urine by application of selected reaction monitoring GC-CI-MS/MS

      Michael Polet, Wim Van Gansbeke, Lore Geldof, Koen Deventer and Peter Van Eenoo

      Version of Record online: 12 MAY 2017 | DOI: 10.1002/dta.2183

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      By using GC-CI-MS/MS, novel long-term metabolites for oxymesterone and mesterolone were detected and characterized. The new oxymesterone metabolite was detectable up to 46 days by using GC-CI-MS/MS, whereas with a traditional screening (detection of metabolite 17-epioxymesterone with GC-EI-MS/MS) oxymesterone administration was only detectable for 3.5 days.

    2. Development of a dried blood spot HPLC-PDA method for the analysis of linezolid and ciprofloxacin in hospital-acquired pneumonia patients

      Vincenzo Ferrone, Maura Carlucci, Roberto Cotellese, Paolo Raimondi, Annadomenica Cichella, Lorenzo Di Marco, Salvatore Genovese and Giuseppe Carlucci

      Version of Record online: 12 MAY 2017 | DOI: 10.1002/dta.2195

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      Development of a dried blood spot technique as an easy tool for the therapeutic drug monitoring of linezolid and cirprofloxacin in patients with hospital acquired pneumonia (HAP).

    3. Distribution pattern of ethyl glucuronide and caffeine concentrations over the scalp of a single person in a forensic context

      Ulf Meier, Thomas Briellmann, Eva Scheurer and Franz Dussy

      Version of Record online: 11 MAY 2017 | DOI: 10.1002/dta.2186

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      A new method for ethyl glucuronide (EtG) measurement in hair using LC–MS3 is described. The extent of variation and distribution of EtG and caffeine concentrations in hair are described across the entire scalp of one volunteer. The implications of the findings for forensic applications of hair analysis are discussed.

    4. Effects of ultrasound irradiation on enzymatic hydrolysis of protein and application for the determination of tetracyclines in complex matrices

      Qian Zhou, Hong Wang, Kuanzheng Zhu, Lihua Zhu, Shengyin Zhou, Jin Peng and Xiya Lu

      Version of Record online: 11 MAY 2017 | DOI: 10.1002/dta.2181

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      The interactions between tetracyclines and protein aggregates are clarified. Effect of various parameters was studied on ultrasound-enhanced enzymatic hydrolysis. Ultrasound changed the secondary structure of trypsin and improved its activity.

    5. Metabolism of the tryptamine-derived new psychoactive substances 5-MeO-2-Me-DALT, 5-MeO-2-Me-ALCHT, and 5-MeO-2-Me-DIPT and their detectability in urine studied by GC–MS, LC–MSn, and LC-HR-MS/MS

      Achim T. Caspar, Jonas B. Gaab, Julian A. Michely, Simon D. Brandt, Markus R. Meyer and Hans H. Maurer

      Version of Record online: 10 MAY 2017 | DOI: 10.1002/dta.2197

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      Studies are described on the metabolism of the NPS 5-methoxy-2-methyl-N,N-diallyltryptamine (5-MeO-2-Me-DALT), 5-methoxy-2-methyl-N-allyl-N-cyclohexyltryptamine (5-MeO-2-Me-ALCHT), and 5-methoxy-2-methyl-N,N-diisopropyltryptamine (5-MeO-2-Me-DIPT) in rat urine or human liver preparations as well as detectability in urine using GC-MS, LC-MSn, and LC-HR-MS/MS. The tryptamines were mainly metabolized by O-demethylation, hydroxylation, N-dealkylation, and combinations of them catalyzed mainly by CYP1A2, CYP2C19, CYP2D6, and CYP3A4 followed by conjugation. In contrast to the GC-MS SUSA, both LC-MS SUSAs were able to detect an intake of 5-MeO-2-Me-ALCHT and 5-MeO-2-Me-DIPT via their metabolites.

  17. Short communications

    1. Return of the lysergamides. Part III: Analytical characterization of N6-ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1-propionyl ETH-LAD (1P–ETH-LAD)

      Simon D. Brandt, Pierce V. Kavanagh, Folker Westphal, Simon P. Elliott, Jason Wallach, Alexander Stratford, David E. Nichols and Adam L. Halberstadt

      Version of Record online: 10 MAY 2017 | DOI: 10.1002/dta.2196

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      N6-Ethyl-6-norlysergic acid diethylamide (ETH-LAD) and 1-propionyl-ETH-LAD, two newly emerging psychoactive lysergamides, were subjected to extensive analytical characterization. A test incubation of 1P–ETH-LAD with human serum at 37°C resulted in the formation of ETH-LAD, suggesting that 1P–ETH-LAD might serve as a pro-drug in vivo.

    2. Ethanol concentration in 56 refillable electronic cigarettes liquid formulations determined by headspace gas chromatography with flame ionization detector (HS-GC-FID)

      Justin L. Poklis, Carl E. Wolf II and Michelle R. Peace

      Version of Record online: 10 MAY 2017 | DOI: 10.1002/dta.2193

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      Fifty-six commercially available e-liquids, purchased from various sources, contained a variety of flavours and active ingredients. A headspace gas chromatography with flame ionization detector (HS-GC-FID) method was used to analyze these e-liquids for volatiles content. Ethanol was determined in 53 of the 56 e-liquids with a range of none detected in five samples to 206 mg/mL.

    3. Increasing the linear dynamic range in LC–MS: is it valid to use a less abundant isotopologue?

      Stephen Trobbiani, Peter Stockham and Timothy Scott

      Version of Record online: 17 APR 2017 | DOI: 10.1002/dta.2175

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      The use of a less abundant isotopologue for quantitation in LC–MS is a simple way to extend the linear dynamic range of a method, especially for high-resolution mass spectrometers. However it may also increase the quantitative error. The likely magnitude of this error was assessed by reviewing the scientific literature for published isotope ratios and the technique was applied to a quantitative LC-TOF method.

  18. Perspectives

    1. Intelligence-based anti-doping from an equine biological passport

      Adam T. Cawley and John Keledjian

      Version of Record online: 17 APR 2017 | DOI: 10.1002/dta.2180

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      The move towards personalized medicine derived from individually-focused clinical chemistry measurements has been translated by the human anti-doping movement over the past decade into developing the athlete biological passport (ABP). There is considerable potential for animal sports to adapt this model to facilitate an intelligence-based anti-doping system.

  19. Research articles

    1. You have free access to this content
      Analysis of drugs of abuse in Cerumen - correlation of postmortem analysis results with those for blood, urine and hair

      Sylvia I. Meier, Sarah C. Koelzer, Manfred Schubert-Zsilavecz and Stefan W. Toennes

      Version of Record online: 12 APR 2017 | DOI: 10.1002/dta.2177

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      Cerumen is a new alternative specimen to prove drug abuse. The time span for the detection of drugs covers not only acute ingestion but also past drug use. The present results suggest a detection time window more than that of urine but not as long as possible with hair. Cerumen is a promising alternative to urine analysis for the assessment of drug abstinence.

    2. Temporal changes in physiology and haematology in response to high- and micro-doses of recombinant human erythropoietin

      Brad Clark, Sarah M. Woolford, Annette Eastwood, Ken Sharpe, Peter G. Barnes and Christopher J. Gore

      Version of Record online: 11 APR 2017 | DOI: 10.1002/dta.2176

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      The temporal response in physiology, performance and athlete biological passport (ABP) parameters to high or high-micro recombinant human erythropoietin dosing regimens was assessed in recreational athletes. The physiological adaptations and modest performance improvements induced by a two week rHuEPO high dose were maintained by rHuEPO micro-dosing for at least three weeks. However, rHuEPO micro-dosing did not mask previous rHuEPO high-dosing and all participants administered rHuEPO registered at least one suspicious ABP value during the administration or washout periods.

    3. Quantification of highly selective sigma-1 receptor antagonist CM304 using liquid chromatography tandem mass spectrometry and its application to a pre-clinical pharmacokinetic study

      Bonnie A. Avery, Pradeep K. Vuppala, Seshulatha Jamalapuram, Abhisheak Sharma, Christophe Mesangeau, Frederick T. Chin and Christopher R. McCurdy

      Version of Record online: 11 APR 2017 | DOI: 10.1002/dta.2156

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      A simple and sensitive UPLC-MS/MS method was developed and validated for the quantification of the novel and highly selective sigma-1 receptor antagonist, CM304, in rat plasma. The newly developed method was successfully applied to a single dose oral (20 mg/kg) and intravenous (2.5 mg/kg) pharmacokinetics study in Sprague Dawley rats. Following the intravenous administration, compound exhibited extravascular distribution (Vd, 5.9 ± 0.1 L/kg) without extra hepatic elimination (CL, 2.0 ± 0.5 L/h/kg) of the CM304.

    4. Structural insights into anticancer activity of D-ring modified estrone derivatives using their lipophilicity in estimation of SAR and molecular docking studies

      Jovana Trifunović, Vladan Borčić, Saša Vukmirović and Momir Mikov

      Version of Record online: 7 APR 2017 | DOI: 10.1002/dta.2172

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      In this research, the QSAR approach was used to examine 14 D-ring modified oestrone derivatives as potential candidates for breast cancer treatment. Examined compounds have been so far considered as aromatase (CYP19A1) inhibitors. The inhibition of oestrogen synthesis is an interesting method for reducing cancer cell multiplication. On the other hand, aromatase inhibitors show high interpatient pharmacokinetic variability, which requires development of new drug candidates.

    5. Enantioselective analysis of citalopram and demethylcitalopram in human whole blood by chiral LC–MS/MS and application in forensic cases

      Sys Stybe Johansen

      Version of Record online: 7 APR 2017 | DOI: 10.1002/dta.2173

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      A chiral liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is developed for the measurement of citalopram and demethylcitalopram enantiomers in whole blood and applied to forensic cases. 7% of the positive citalopram cases would be toxicological misinterpretated if chirality was not determined.

  20. Reviews

    1. Challenges in detecting substances for equine anti-doping

      A. G. Fragkaki, N. Kioukia-Fougia, P. Kiousi, M. Kioussi and M. Tsivou

      Version of Record online: 5 APR 2017 | DOI: 10.1002/dta.2162

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      In equine anti-doping, the detection of an enormous number of prohibited substances (or methods) must be controlled compared to those in human sports, as the health of two individuals must be protected: the human's and the horse's. Diverse drug classes must be analyzed in multi-targeted methods with a minimal drop in sensitivity. The use of innovative techniques, such as omics, and the evolution of instrumental techniques offer a powerful contribution to the fight for clean equine sports.

  21. Research articles

    1. Microbial biotransformation of five pyrrolidinophenone-type psychoactive substances in wastewater and a wastewater isolated Pseudomonas putida strain

      Marie Mardal, Markus Bischoff, María Ibáñez, Ulla Ruffing, Félix Hernández and Markus R. Meyer

      Version of Record online: 4 APR 2017 | DOI: 10.1002/dta.2165

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      A Pseudomonas putida strain isolated from MDPV-enriched wastewater reproducibly produced transformation products (TPs) of five pyrrolidinophenone-type psychoactive substances, including alkyl hydroxylations and subsequent N-desalkyl and oxidation. Additionally, wastewater-incubations of the same substances revealed identical and additional TPs. The overlapping pathway indicates this isolated strain can be useful for identification of microbial TPs for wastewater-based epidemiology.

    2. An exploratory study Evaluating the impact of opioid and non-opioid pain medications on serum/plasma free testosterone and free estradiol concentrations

      Julie A. Ray, Mark M. Kushnir, A. Wayne Meikle, Jill E. Sindt and Frederick G. Strathmann

      Version of Record online: 31 MAR 2017 | DOI: 10.1002/dta.2174

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      This paper explores the influence of opioid and non-opioid pain medications on concentrations of free testosterone and free oestradiol. Particular opioid medications such as methadone, tramadol, or fentanyl, and non-opioid medications such as pregabalin or gabapentin, may offer advantages over other opioid medications for treating pain with fewer side effects.

    3. Rapid classification and quantification of cocaine in seized powders with ATR-FTIR and chemometrics

      Joy Eliaerts, Pierre Dardenne, Natalie Meert, Filip Van Durme, Nele Samyn, Koen Janssens and Karolien De Wael

      Version of Record online: 31 MAR 2017 | DOI: 10.1002/dta.2149

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      ATR-FTIR spectrometry combined with SVM resulted in a significant upgrade of the screening test to a reliable and straightforward classification and quantification tool for cocaine in seized drug powders. The entire process of classification (cocaine detected or cocaine not detected) and a reliable estimation of the cocaine content can be completed within less than four minutes per sample, emphasizing its potential for high throughput and on-site applications.

    4. The role of diode array ultraviolet detection for the identification of synthetic cathinones

      Walter F. Rowe, Ioan Marginean, Stephanie Carnes and Ira S. Lurie

      Version of Record online: 15 MAR 2017 | DOI: 10.1002/dta.2163

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      The utility of diode array UV detection for aiding in the identification of synthetic cathinones, including different sub classes and positional isomers is presented. There was at least a 10 nm hypsochromic shift in UV maximum (shift to shorter wavelengths) for UHPSFC versus reversed phase ultra-high performance liquid chromatography (UHPLC).

    5. Racing chemistry: A century of challenges and progress

      Christopher Kremmer

      Version of Record online: 8 MAR 2017 | DOI: 10.1002/dta.2147

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      Jean Kimble peering into a microscope with camera attachment and the official group portrait taken at the AORC's second annual conference, held on May 18, 1949 in New York City. Kimble is standing in the middle row fifth from the left. The woman next to her, who is dressed in darker clothing is another female scientist of that era, Elsie Bellows. The man sitting in the front row, third from the right is Charles Morgan, the AORC President at the time.

  22. Short communications

    1. Characterization of hallucinogenic phenethylamines using high-resolution mass spectrometry for non-targeted screening purposes

      Daniel Pasin, Adam Cawley, Sergei Bidny and Shanlin Fu

      Version of Record online: 8 MAR 2017 | DOI: 10.1002/dta.2171

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      Hallucinogenic phenethylamines such as 2,5-dimethoxyphenethylamines (2C–X), their N-(2-methoxybenzyl) derivatives (25X–NBOMe) and 2,5-dimethoxyphenethylamines were characterized using UPLC-QTOF-MS. Common product ions and neutral losses were identified which can be utilized to detect noel analogues.

  23. Research articles

    1. Intracerebral microdialysis coupled to LC–MS/MS for the determination tramadol and its major pharmacologically active metabolite O-desmethyltramadol in rat brain microdialysates

      Mingzhou Liu, Peng Wang, Xuming Yu, Guicheng Dong and Jiang Yue

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/dta.2157

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      A simple and sensitive LC-ESI-MS/MS coupled to Intracerebral microdialysis method coupled to an intracerebral microdialysis technique was developed for the simultaneous determination of tramadol and its major active metabolite O-desmethyltramadol in rat brain. The proposed method was successfully applied to the pharmacokinetic studys of tramadol and ODT in rat brain.

    2. Pharmacokinetics of betamethasone in plasma, urine, and synovial fluid following intra-articular administration to exercised thoroughbred horses

      Heather K. Knych, Scott D. Stanley, Linda M. Harrison and Daniel S. Mckemie

      Version of Record online: 7 MAR 2017 | DOI: 10.1002/dta.2170

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      Following intra-articular administration to exercised Thoroughbred horses, betamethasone was detected for up to 96 h and 7 days in plasma and urine, respectively. Betamethasone fell below detectable levels in synovial fluid between 14 and 21 days post administration and therefore urine and blood concentrations do not appear to be good indicators of drug concentrations at the effector site and by extrapolation may not be useful in determining the duration of pharmacologic effect.

    3. Identification of gonadotropin-releasing hormone metabolites in greyhound urine

      David Palmer, Katie Rademaker, Ingrid Martin, Joan Hessell and Rob Howitt

      Version of Record online: 3 MAR 2017 | DOI: 10.1002/dta.2164

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      An administration study of gonadotropin-releasing hormone in greyhounds revealed three novel metabolites in urine. Two of these metabolites are relatively stable in urine, allowing enhanced ability to detect gonadotropin-releasing hormone abuse in canine athletes.

    4. You have full text access to this OnlineOpen article
      A sensitive assay for urinary cocaine metabolite benzoylecgonine shows more positive results and longer half-lives than those using traditional cut-offs

      Joyce Nickley, Amadeo J. Pesce and Kevin Krock

      Version of Record online: 3 MAR 2017 | DOI: 10.1002/dta.2153

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      A sensitive assay for urinary cocaine metabolite benzoylecgonine shows more positive results and longer half-lives than those using traditional cut-offs.

    5. Creatinine in urine – a method comparison

      Marc Luginbühl and Wolfgang Weinmann

      Version of Record online: 3 MAR 2017 | DOI: 10.1002/dta.2166

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      Three different methods for the determination of creatinine concentrations in urine are carefully investigated. LC–MS/MS proved to be advantageous compared to a spectrophotometric or point-of-care testing based analysis method.

    6. Identification of novel disulfide adducts between the thiol containing leaving group of the nerve agent VX and cysteine containing tripeptides derived from human serum albumin

      Andreas Kranawetvogl, Jim Küppers, Michael Gütschow, Franz Worek, Horst Thiermann, Paul W. Elsinghorst and Harald John

      Version of Record online: 3 MAR 2017 | DOI: 10.1002/dta.2144

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      Recently, phosphonylated tyrosine residues and disulfide adducts between the leaving group of the nerve agent VX (2-(diisopropylamino)ethanethiol, DPAET) and cysteine containing dipeptides were detected simultaneously using μLC-ESI MS/HR MS after pronase cleavage of incubated human serum albumin (HSA). Accordingly, we herein present two novel tripeptides representing HSA-disulfide adducts with DPAET (Met-Pro-Cys-DPAET, MPC-DPAET and Asp-Ile-Cys-DPAET, DIC-DPAET). The limit of detection for MPC-DPAET revealed toxicologically relevant VX plasma concentrations, which provided novel insights into the reactivity of VX and its endogenous targets.

    7. Evaluation of KIMS immunoassays on a cobas c 501 analyzer for drugs of abuse and ethyl glucuronide testing in urine for forensic abstinence control

      Merja A. Neukamm, Arsham Bahrami, Volker Auwärter, Felix M.P. Mehne and Eva Höss

      Version of Record online: 24 FEB 2017 | DOI: 10.1002/dta.2154

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      Drugs of abuse immunoassays (KIMS, DRI) for urine screening were evaluated on a cobas c 501 using authentic urine samples and quality controls. Relative standard deviation and bias were below 12%, onboard calibration stability was in the range of 21 to 28 days, cross reactivity was determined for a number of new psychoactive substances, sensitivity was 100% for all analytes except EDDP, and specificity was below 90% for amphetamines and benzodiazepines only. The immunoassays fulfil the requirements for forensic abstinence control.

    8. Identification and analytical characterization of six synthetic cannabinoids NNL-3, 5F–NPB-22-7N, 5F–AKB-48-7N, 5F–EDMB-PINACA, EMB-FUBINACA, and EG-018

      Cuimei Liu, Wei Jia, Zhendong Hua and Zhenhua Qian

      Version of Record online: 24 FEB 2017 | DOI: 10.1002/dta.2160

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      Three indazole 7N positional isomer synthetic cannabinoids of NNL-3, 5F–NPB-22-7N, and 5F–AKB-48-7N; two ethyl 2-amino-3-methylbutanoate-type synthetic cannabinoids of 5F–EDMB-PINACA and EMB-FUBINACA; and one 9H–carbazole substituted synthetic cannabinoid of EG-018 were identified using UHPLC-QTOF-MS, GC–MS, NMR, and IR.

    9. In vitro phase I metabolism of selective estrogen receptor modulators in horse using ultra-high performance liquid chromatography-high resolution mass spectrometry

      Karen Y. Kwok, George H. M. Chan, Wai Him Kwok, Jenny K. Y. Wong and Terence S. M. Wan

      Version of Record online: 16 FEB 2017 | DOI: 10.1002/dta.2158

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      Identification of in vitro phase I metabolites of tamoxifen and toremifene as potential screening targets for the detection of their misuses in racehorces. N-Hydroxymethylated metabolites were first reported in equine.

    10. Doping control analysis of lithium in horse urine and plasma by inductively coupled plasma mass spectrometry

      Timmy L. S. Choi, Jenny K. Y. Wong, Emmie N. M. Ho, Wai Him Kwok, Gary N. W. Leung, Peter Curl and Terence S. M. Wan

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2159

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      Lithium salts are commonly prescribed to treat bipolar disorder in humans. As they have mood-stabilizing effect and are orally active and inexpensive, lithium salts are attractive doping agents in equine sports. This paper describes the validation of quantification methods for lithium in equine urine and plasma using inductively coupled plasma mass spectrometry (ICP-MS). Population studies of lithium in horse urine and horse administration studies of lithium chloride were carried out. A urinary threshold of lithium was proposed based on these studies.

    11. Persistence of alprazolam in river water according to forced and non-forced degradation assays: adsorption to sediment and long-term degradation products

      Juan J. Jiménez, María I. Sánchez, Beatriz E. Muñoz and Rafael Pardo

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2148

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      Biological, photochemical and thermal degradation of alprazolam in river water is negligible under forced and non-forced conditions. Tentative structures for 8 out of 9 long-term degradation products are proposed from high-resolution tandem mass-spectrometry data. Alprazolam can be adsorbed onto aquatic sediment.

  24. Short communications

    1. Alpha-PVP as an active component of herbal highs in Poland between 2013 and 2015

      Bogumiła Byrska, Roman Stanaszek and Dariusz Zuba

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2151

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      This paper is a review analysis of cases in which alpha-PVP was identified in herbal samples seized during 2013–2015 in Poland. The study showed high heterogeneity of qualitative and quantitative composition of identically labelled products, carrying a great risk of unpredictable toxic effects.

  25. Research articles

    1. Profiling and identification of (−)-epicatechin metabolites in rats using ultra-high performance liquid chromatography coupled with linear trap-Orbitrap mass spectrometer

      Zhanpeng Shang, Fei Wang, Shengyun Dai, Jianqiu Lu, Xiaodan Wu and Jiayu Zhang

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2155

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      A strategy based on urtra-high-performance liquid chromatography coupled with linear ion trap-Orbitrap mass spectrometer has been developed to comprehensive identify EC in vivo metabolites. Meanwhile, the metabolic pathway of EC was proposed according to the detected 67 metabolites.

    2. Detection and in vitro metabolism of the confiscated peptides BPC 157 and MGF R23H

      Holly D. Cox, Geoff D. Miller and Daniel Eichner

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2152

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      The peptide BPC 157 was identified in confiscated vials and methods were developed for its detection in urine. The primary metabolite was identified and measured using in vitro methods.

    3. In vitro studies on flubromazolam metabolism and detection of its metabolites in authentic forensic samples

      Carolina Noble, Marie Mardal, Niels Bjerre Holm, Sys Stybe Johansen and Kristian Linnet

      Version of Record online: 10 FEB 2017 | DOI: 10.1002/dta.2146

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      Flubromazolam is adesigner benzodiazepine first detected as an abused drug in 2014. By using various in vitro system, we identified CYP3A4 and CYP3A5 as the main contributing CYP enzymes in mediating the (x-hydrody- (M1), 4-hydrody- (M2) and(a,4)–dihydroxy-flubromazolam (M3) in human liver microsomes (pHLM). Analysis of authentic samples revealed flubromazolam, M1 and the subsequently glucuronidated metabolite (M5), as well as the directly N-glucuronidated flubromazolam (M6) to be excreted in urine, while M2 and the corresponded glucuronide (M4) were not detected in this specimen. Finally, further studies showed flubromazolam is a highly protein-bound drug with a predicted low clearance.

    4. A genetic algorithm-based framework for wavelength selection on sample categorization

      Michel J. Anzanello, Gabrielli Yamashita, Marcelo Marcelo, Flávio S. Fogliatto, Rafael S. Ortiz, Kristiane Mariotti and Marco F. Ferrão

      Version of Record online: 7 FEB 2017 | DOI: 10.1002/dta.2138

      Thumbnail image of graphical abstract

      A novel framework for selecting the most relevant subsets of wavelengths for classification of samples into two classes using KNN and genetic algorithm was developed. Intervals yielding high classification accuracies in KNN were refined through genetic algorithm by identifying a limited number of wavelengths aimed at maximizing classification accuracy. A remarkable reduction in the number of retained wavelengths and an increase of the classification accuracy were achieved.

  26. Short communications

    1. Application of HBOCs electrophoretic method to detect a new blood substitute derived from the giant extracellular haemoglobin of lugworm

      A. Marchand, N. Crepin, I. Roulland, F. Semence, V. Domergue, F. Zal, V. Polard and A. Coquerel

      Version of Record online: 13 JAN 2017 | DOI: 10.1002/dta.2127

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      The aim of this work was to test the capacity of detection of a new kind of haemoglobin-based oxygen carrier (HBOC) issued from a marine worm. The electrophoretic method used for detection of the first-generation HBOC was applied. The highlights of this work are:

      • HEMOXYCarrier® produced by HEMARINA is a future blood substitute with doping potential.
      • Detection of this product in plasma/serum using the electrophoretic HBOC method is applicable but limited in vivo to a few hours.
      • Research of peptides specific of worm globins in blood or urine could increase the window of detection.
    2. Enantioselective disposition of (R)-salmeterol and (S)-salmeterol in urine following inhaled dosing and application to doping control

      Glenn A. Jacobson, Morten Hostrup, Christian K. Narkowicz, David S. Nichols and E. Haydn Walters

      Version of Record online: 29 DEC 2016 | DOI: 10.1002/dta.2131

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      • Salmeterol is restricted by the World Anti-Doping Agency (WADA), with inhalation permitted within predetermined dosing threshold.
      • There is currently no equivalent urine threshold for salmeterol, which is made difficult due to the very low levels of drug observed in urine.
      • Racemic salmeterol delivered by inhalation exhibits enantioselectivity in urine and levels can be detected in urine up to 24 hours after dosing with either 50 or 200 µg inhaled dosing.
  27. Research articles

    1. Identification of porcine relaxin in plasma by liquid chromatography-high resolution mass spectrometry

      April S. Y. Wong, Emmie N. M. Ho, W. H. Kwok, Gary N. W. Leung, Yuehong Shen, Robert Z. Qi, Samuel K. Yue and Terence S. M. Wan

      Version of Record online: 28 DEC 2016 | DOI: 10.1002/dta.2143

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      Relaxin is an insulin-like protein with multiple and diverse pharmacological functions. Intelligence has shown that RLX has already been abused to improve racehorse performance. A sensitive and selective method for the identification of pRLX in equine plasma is presented in this paper.

    2. Applicability of ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry for cocaine profiling

      Cuimei Liu, Zhendong Hua and Xin Meng

      Version of Record online: 28 DEC 2016 | DOI: 10.1002/dta.2132

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      A UHPLC-QTOF-MS method for analysis of 14 cocaine alkaloid impurities and statistical methodology for cocaine profiling were established and validated. After hierarchical cluster analysis (HCA), 183 cocaine samples collected from 2011 to 2015 were classified into 7 major groups. Moreover, 37 groups of linked samples were found within and between provinces, which provide intelligence for the case connection and revealing of the distribution networks.

    3. Identification and analytical characterization of nine synthetic cathinone derivatives N-ethylhexedrone, 4-Cl-pentedrone, 4-Cl-α-EAPP, propylone, N-ethylnorpentylone, 6-MeO-bk-MDMA, α-PiHP, 4-Cl-α-PHP, and 4-F-α-PHP

      Cuimei Liu, Wei Jia, Tao Li, Zhendong Hua and Zhenhua Qian

      Version of Record online: 28 DEC 2016 | DOI: 10.1002/dta.2136

      Thumbnail image of graphical abstract

      Nine synthetic cathinone derivatives N-ethylhexedrone, 4-Cl-pentedrone, 4-Cl-α-EAPP, propylone, N-ethylnorpentylone, 6-MeO-bk-MDMA, α-PiHP, 4-Cl-α-PHP, and 4-F-α-PHP were identified using UHPLC-QTOF-MS, GC-MS, and NMR. The mass-spectral fragmentations of these compounds following collision-induced dissociation (CID) and electron ionization (EI) were studied to assist forensic laboratories in identifying these compounds or other substances with similar structure in their case work.

    4. Freeze-thaw stability and long-term stability of 84 synthetic cannabinoids in serum

      Cornelius Hess, Lynn Krueger, Michael Unger and Burkhard Madea

      Version of Record online: 28 DEC 2016 | DOI: 10.1002/dta.2133

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      Synthetic cannabinoids seem to be very stable after three freeze-and thaw cycles and regarding long-term stability. For 82 of 84 tested substances stability in serum could be shown for at least 1 month at -20°C.

    5. Targeted analysis of 116 drugs in hair by UHPLC-MS/MS and its application to forensic cases

      Xin Wang, Sys Stybe Johansen, Marie Katrine Klose Nielsen and Kristian Linnet

      Version of Record online: 22 DEC 2016 | DOI: 10.1002/dta.2130

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      A multi-target method that can quantify a broad range of drugs and drugs of abuse (116 drugs) with high sensitivity in human hair using UHPLC–MS/MS was developed with a good performance in the validation. The applicability of the method was demonstrated by the analysis of forensic postmortem cases.

    6. Preclinical pharmacokinetics and ADME characterization of a novel anticancer chalcone, cardamonin

      Swati Jaiswal, Mahendra Shukla, Abhisheak Sharma, Nagarjun Rangaraj, Kalpesh Vaghasiya, Mohd Yaseen Malik and Jawahar Lal

      Version of Record online: 28 NOV 2016 | DOI: 10.1002/dta.2128

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      An array of in situ, in vitro, and in vivo studies was carried out for pre-clinical ADME characterization of cardamonin, which would be helpful for its development as potential anti-cancer drug.

  28. Reviews

    1. A review of designer anabolic steroids in equine sports

      Christopher C. Waller and Malcolm D. McLeod

      Version of Record online: 18 NOV 2016 | DOI: 10.1002/dta.2112

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      Designer steroids pose a growing threat to the integrity of equine sports. Studies of the in vivo and in vitro metabolism of designer steroids in equine systems are critically reviewed, highlighting recommended target analytes, analytical approaches, and future directions.

  29. Research articles

    1. DNA typing for personal identification of urine after long-term preservation for testing in doping control

      Kimiko Aoki, Hiroyuki Tanaka and Makoto Ueki

      Version of Record online: 18 NOV 2016 | DOI: 10.1002/dta.2126

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      To cope with a case that the tampering of a urine sample is suspected in doping control, we established a urinary DNA extraction method suitable for the personal identification by STR analysis. The success ratio of STR analysis using 30 mL of urine samples from men cryopreserved for 3–7 years was at least 86%.

    2. Comparative evaluation of chemical profiles of three representative 'snow lotus' herbs by UPLC-DAD-QTOF-MS combined with principal component and hierarchical cluster analyses

      Qi-Lei Chen, Lin Zhu, Yi-Na Tang, Hiu-Yee Kwan, Zhong-Zhen Zhao, Hu-Biao Chen and Tao Yi

      Version of Record online: 18 NOV 2016 | DOI: 10.1002/dta.2123

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      An UPLC-DAD-QTOF-MS method was developed and used to analyze 49 herbal samples for species analysis and overall quality evaluation. 4D-PCA and 2D-HCA results illustrated that Saussurea laniceps (SL) should be grouped away from Saussurea medusa (SM) and Saussurea involucrata (SI), contradicting the record in Flora of China.

    3. Application of testosterone to epitestosterone ratio to horse urine – a complementary approach to detect the administrations of testosterone and its pro-drugs in Thoroughbred geldings

      Marjaana Viljanto, James Scarth, Pamela Hincks, Lynn Hillyer, Adam Cawley, Craig Suann, Glenys Noble, Christopher J. Walker, Andrew T. Kicman and Mark C. Parkin

      Version of Record online: 11 NOV 2016 | DOI: 10.1002/dta.2109

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      The use of steroid ratios may provide a supplementary approach to aid in differentiating the administration of testosterone and its pro-drugs and unusual conditions resulting in elevated testosterone concentrations in geldings. In the current study, an upper limit of 5 was proposed for the ratio of urinary testosterone: epitestosterone (T:E). Analysis of atypical urine samples showed that the T:E ratio remained below the proposed limit, whilst it was exceeded following the administration of a range of separate testosterone-related steroids.

    4. Control of methylxanthines in the competition horse: pharmacokinetic/pharmacodynamic studies on caffeine, theobromine and theophylline for the assessment of irrelevant concentrations

      Marc Machnik, Simone Kaiser, Sophie Koppe, Manfred Kietzmann, Ina Schenk, Michael Düe, Mario Thevis, Wilhelm Schänzer and Pierre-Louis Toutain

      Version of Record online: 4 NOV 2016 | DOI: 10.1002/dta.2097

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      Methylxanthines are naturally occuring prohibited substances necessitating an adequate consideration in doping control by racing and equestrian authorities. However, international rules for the control of methylxanthines are in place for theobromine only. The present paper attempts to assist racing laboratories and authorities in reporting and interpreting methylxanthines findings in a transparent, consistent and defensible manner. Therefore PK/PD studies were carried out including i.v. and oral administrations of caffeine, theobromine and theophylline. Plasma and urine concentrations were determined by LC-MS/MS. Toutain modelling on the obtained data was applied to investigate irrelevant concentrations of methylxanthines in the horse. These irrelevant concentrations were used to propose international residue limits for methylxanthines in the competition horse.

    5. Confirmatory analysis of etanercept in equine plasma by LC-MS for doping control

      Fuyu Guan, Mary A. Robinson and Lawrence R. Soma

      Version of Record online: 5 OCT 2016 | DOI: 10.1002/dta.2091

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      The present study has established an LC-MS method for confirmation of etanercept in equine plasma. This is the first reported method for confirmation of etanercept in plasma by LC-MS.

    6. Doping control analysis of anabolic steroids in equine urine by gas chromatography-tandem mass spectrometry

      April S. Y. Wong, Gary N. W. Leung, David K. K. Leung and Terence S. M. Wan

      Version of Record online: 5 OCT 2016 | DOI: 10.1002/dta.2090

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      A sensitive method was developed for the simultaneous detection of 52 steroids in equine urine using GC-MS/MS. The developed method has enhanced sensitivity and selectivity for detection of free and conjugated steroids. It has acceptable precision and recovery to be used as a qualitative screening method on a regular basis.

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