Drug Testing and Analysis

Cover image for Vol. 5 Issue 6

June 2013

Volume 5, Issue 6

Pages i–i, 384–508

  1. Cover picture

    1. Top of page
    2. Cover picture
    3. Research articles
    1. Cover Picture (page i)

      Article first published online: 11 JUN 2013 | DOI: 10.1002/dta.1495

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  2. Research articles

    1. Top of page
    2. Cover picture
    3. Research articles
    1. A quantitative approach for assessing significant improvements in elite sprint performance: Has IGF-1 entered the arena? (pages 384–389)

      Simon Ernst and Perikles Simon

      Article first published online: 29 AUG 2012 | DOI: 10.1002/dta.1406

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      The introduction of doping substances and methods in sports are supposed to trigger noticeable effects on physical performances in metric sports. Here, we use time series analysis to investigate the recent development in male and female elite sprinting performance.

    2. Comparison of LUCIO®-direct ELISA with CEDIA immunoassay for ‘zero tolerance’ drug screening in urine as required by the German re-licensing guidelines (pages 390–399)

      Ronald Agius, Thomas Nadulski, Hans-Gerhard Kahl and Bertin Dufaux

      Article first published online: 24 JAN 2013 | DOI: 10.1002/dta.1455

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      Relative sensitivities and relative specificities were calculated at 99.7 % and 98.4 % for direct ELISA and 66 % and 91.4 % for CEDIA respectively for drugs of abuse screening when applied to the German abstinence cut-offs at 10 ng/mL cannabinoids, 50 ng/mL amphetamines and designer amphetamines, 25 ng/mL opiates, 30 ng/mL cocaine metabolite, 50 ng/mL methadone metabolite and benzodiazepines at 50 ng/mL in urine.

    3. Standardless 1H NMR determination of pharmacologically active substances in dietary supplements and medicines that have been illegally traded over the Internet (pages 400–411)

      Yulia B Monakhova, Thomas Kuballa, Sigrid Löbell-Behrends, Sibylle Maixner, Matthias Kohl-Himmelseher, Winfried Ruge and Dirk W Lachenmeier

      Article first published online: 1 MAY 2012 | DOI: 10.1002/dta.1367

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      400 MHz 1H NMR spectroscopy is used to detect pharmacologically active substances in food supplements and medicines, which are widely marketed in an illegal or counterfeited way over the Internet. An example is sibutramine in anorectic formulations such as so-called slimming tea. The NMR approach has the advantage that identification and quantification is often possible, even when pure compounds as reference standards are unavailable.

    4. Metabolic studies of formestane in horses (pages 412–419)

      Gary N. W. Leung, W. H. Kwok, Terence S. M. Wan, Kenneth K. H. Lam and Peter J. Schiff

      Article first published online: 21 JAN 2013 | DOI: 10.1002/dta.1444

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      Formestane, a steroidal aromatase inhibitor, can be used for building muscles by stopping the conversion of testosterone into estradiol, resulting in the increase of testosterone level in the body. While it was banned in human and equine sports, little is known about its metabolic fate in horses. This paper describes the metabolic studies of formestane in horses, with an aim to identify the most appropriate target metabolites to be monitored for controlling the misuse or abuse of formestane in racehorses.

    5. Prevalence and co-existence of active components of ‘legal highs’ (pages 420–429)

      Dariusz Zuba and Bogumiła Byrska

      Article first published online: 1 MAY 2012 | DOI: 10.1002/dta.1365

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      The results of a study performed on samples of ‘legal highs’ seized in ‘head shops’ in Poland between mid-2008 and mid-2011 were presented. The most common ingredients were MPDV, caffeine, butylone, TFMPP, lidocaine, 4-MEC, mephedrone, pFPP, BZP and MDPBP. Cathinones and piperazines were mixed mainly within the chemical classes, caffeine was mixed both with piperazines and cathinones, whereas lidocaine only with the latter class. A great inconsistency in the qualitative and quantitative composition of products with identical labelling was shown.

    6. In vitro metabolism studies on mephedrone and analysis of forensic cases (pages 430–438)

      Anders Just Pedersen, Lotte Ask Reitzel, Sys Stybe Johansen and Kristian Linnet

      Article first published online: 9 MAY 2012 | DOI: 10.1002/dta.1369

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      Mephedrone is a designer-drug that has gained increasing use in recent years. In vitro studies showed that the main enzyme responsible for metabolism of mephedrone was cytochrome P450 2D6, which formed hydroxytolyl- and nor-mephedrone, of which the former was purified and identified by NMR. In forensic cases, these metabolites and 4-carboxy-dihydro-mephedrone were identified by LC-MS/MS and LC-TOF in blood or urine, additionally, two previously unreported metabolites, dihydro-mephedrone and 4-carboxy-mephedrone were detected.

    7. An evaluation of the DRI-ETG EIA method for the determination of ethyl glucuronide concentrations in clinical and post-mortem urine (pages 439–445)

      Sophie C. Turfus, Tu Vo, Nadia Niehaus, Dimitri Gerostamoulos and Jochen Beyer

      Article first published online: 28 FEB 2012 | DOI: 10.1002/dta.414

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      The performance of a commercial immunoassay for detection of ethyl glucuronide in urine is evaluated against a liquid chromatography tandem mass spectrometry method. The use of the immunoassay for qualitative and quantitative determinations is appraised in the context of both post-mortem and clinical samples (n=1000). The immunoassay gives a very good approximation to the EtG concentration in both sample types and its use as a more economic alternative can be justified with no detrimental effect on the determined EtG concentration.

    8. Concentrations of atomoxetine and its metabolites in plasma and oral fluid from paediatric patients with attention deficit/hyperactivity disorder (pages 446–452)

      Esther Papaseit, Emilia Marchei, Magí Farré, Oscar Garcia-Algar, Roberta Pacifici and Simona Pichini

      Article first published online: 15 MAY 2012 | DOI: 10.1002/dta.1370

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      Atomoxetine (ATX) is a non-stimulant drug approved for the treatment of children and adolescents with attention deficit/hyperactivity disorder (ADHD). We studied the excretion profile of ATX and its principal metabolites 4-hydroxyatomoxetine (4-OH-ATX) and N-desmethylatomoxetine (desmethyl-ATX) in oral fluid and plasma of ADHD paediatric subjects, after administration of different dosage regimens.

      The correlations between ATX and 4-OH-ATX concentrations in plasma and oral fluid indicate that oral fluid concentrations of this drug and its principal metabolite may be a predictor of plasma concentrations, even if values are too low and variable to be considered an alternative to plasma.

    9. Bioanalytical method development, pharmacokinetics, and toxicity studies of paromomycin and paromomycin loaded in albumin microspheres (pages 453–460)

      Wahid Khan, Shyam S. Sharma and Neeraj Kumar

      Article first published online: 22 MAR 2012 | DOI: 10.1002/dta.339

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      Paromomycin loaded albumin microspheres were prepared to target Paromomycin to macrophages. A new bioanalytical method was developed and found to be very sensitive. Pharmacokinetic studies performed in rat showed reduction in Cmax of free Paromomycin when administered as developed microsphere formulation. Toxicity studies indicated better toxicity profile for prepared formulation as compared to marketed Paromomycin IM injection for the treatment of visceral leishmaniasis.

    10. A biomimetic potentiometric sensor based on molecularly imprinted polymer for the determination of memantine in tablets (pages 461–467)

      Majid Arvand and Hedyeh Asadi Samie

      Article first published online: 18 APR 2012 | DOI: 10.1002/dta.371

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      Molecularly imprinted polymers (MIPs) exhibiting high selectivity and affinity to the predetermined molecule are now seeing a fast growing research

    11. Paromomycin-loaded albumin microspheres: Efficacy and stability studies (pages 468–473)

      Wahid Khan, Rajendra Kumar, Sukhvinder Singh, Sunil Kumar Arora and Neeraj Kumar

      Article first published online: 18 APR 2012 | DOI: 10.1002/dta.389

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      Paromomycin-loaded albumin microspheres were formulated and tested for efficacy and stability in present work. Efficacy studies provided significant increase in efficacy of formulation in comparison to PM solution at equivalent concentration. Stability studies proved stability of prepared microsphere formulation at all tested conditions including accelerated conditions.

    12. Monitoring of aglycons of yew glycosides (3,5-dimethoxyphenol, myrtenol and 1-octen-3-ol) as first indicator of yew presence (pages 474–479)

      V. Varlet and M. Augsburger

      Article first published online: 28 FEB 2012 | DOI: 10.1002/dta.391

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      The detection of 3,5-dimethoxyphenol (3,5-DMP), myrtenol and 1-octen-3-ol compounds is easily performed by GC-MS (SIM) after an enzymatic hydrolysis (β-glucosidase) allowing the release of volatile compounds from yew glycosides. Their presence and relative amount consitute key indicators to confirm a yew ingestion.

    13. Study on the aconitine-type alkaloids of Radix Aconiti Lateralis and its processed products using HPLC-ESI-MSn (pages 480–484)

      Yonggang Liu, Peng Tan, Fei Li and Yanjiang Qiao

      Article first published online: 22 MAR 2012 | DOI: 10.1002/dta.416

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      The alkaloids of Radix Aconiti Lateralis were studied. 48 compounds were structurally identified, among them, a new kind of alkaloids was found with protonated molecules at m/z 452, 468 and 482.

    14. Development and validation of an HPLC-UV method for simultaneous determination of zidovudine, lamivudine, and nevirapine in human plasma and its application to pharmacokinetic study in human volunteers (pages 485–491)

      Utpal Nandi, Ayan Das, Bikash Roy, Hira Choudhury, Bapi Gorain and Tapan Kumar Pal

      Article first published online: 28 FEB 2012 | DOI: 10.1002/dta.419

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      A simple, feasible, cost effective, rapid accurate, specific and sensitive high-performance liquid chromatographic method with UV detection has been developed and validated according to the FDA guidelines for the determination of zidovudine, lamivudine and nevirapine in human plasma. It was successfully applied to analyze the plasma samples of the pharmacokinetic study of the above drugs formulations in 12 healthy human volunteers.

    15. Determination of febuxostat in human plasma using ultra-performance liquid chromatography tandem mass spectrometry (pages 492–499)

      Ojikumar Lukram, Shivaji Parmar and Amit Hande

      Article first published online: 15 MAR 2012 | DOI: 10.1002/dta.420

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      A rapid and sensitive liquid chromatography tandem mass spectrometry method has been developed and validated for the determination of febuxostat in human plasma. The liquid–liquid extraction technique was used for the extraction of febuxostat from human plasma using trandolapril as the internal standard (IS). Chromatography was performed on a UPLC BEH C18, 50 mm X 2.1 mm, 1.7 µm particle size column, with the mobile phase consisting of 0.1% formic acid and acetonitrile (in a 25:75 ratio), followed by detection using mass spectrometry. The method involves a simple reversed isocratic chromatography condition and mass spectrometry detection, which enables detection at sub-microgram levels. The method was validated and the lower limit of quantification for febuxostat was found to be 0.075 µg/mL. The mean recovery for febuxostat ranged from 100.92 to 106.5%. This method increased the sensitivity and selectivity; resulting in high-throughput analysis of febuxostat using commercially available IS for pharmacokinetic, bioavailability and bioequivalence studies, with a chromatographic run time of 1.5 min only.

    16. A validated HPLC method for the simultaneous determination of naftidrofuryl oxalate and its degradation product (metabolite), naftidrofuryl acid: applications to pharmaceutical tablets and biological samples (pages 500–508)

      Suzy M. Sabry, Tarek S. Belal, Magda H. Barary and Mohammed E. A. Ibrahim

      Article first published online: 28 FEB 2012 | DOI: 10.1002/dta.421

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      A simple, sensitive and selective RP-HPLC method was described for the simultaneous determination of naftidrofuryl oxalate (NF) and its hydrolytic degradation product (metabolite), naftidrofuryl acid (NFA). The method was applied as a stability-indicating assay of the parent drug NF in its tablets. Also, the degradation product NFA was determined down to a level of 0.005% in presence of large excess of the parent drug. Finally, drug monitoring of NF and its metabolite in human plasma/urine samples was carried out.