Annual banned-substance review Research articles Contents continued overleaf 8(1) (2016) ISSN

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1 1 Volume 8 Number 1, January 2016 Annual banned-substance review Detection assays for drugs and methods of sports doping published between 2014 and 2015 are critically reviewed and evaluated in context with the Prohibited List 2015 as established by the World Anti-Doping Agency. Annual banned-substance review: analytical approaches in human sports drug testing 7 29 M. Thevis, T. Kuuranne, K. Walpurgis, H. Geyer and W. Schänzer Research articles The development of the first fully automated method for the determination of opioids in dried blood spots is described. Selective, sensitive, accurate, and reproducible quantitation of five representative opioids at sub therapeutic, therapeutic, and toxic levels can be achieved within 5 min. Quantitative determination of opioids in whole blood using fully automated dried blood spot desorption coupled to on line SPE LC MS/MS R. Verplaetse and J. Henion Comprehensive UHPLC HR TOF MS based confirmation level screening was employed to determine the accurate drug abuse patterns of drug users with different attendance for drug treatment. Those subjects regularly attending treatment mainly abused medicinal buprenorphine and benzodiazepines. Conversely, the conventional illicit drugs amphetamine and cannabis were more frequent among the subjects irregularly attending treatment, together with a higher rate of new psychoactive substances and polydrug abuse. Treatment of drug abusers thus could be valuable in reducing polydrug abuse. Patterns of drug abuse among drug users with regular and irregular attendance for treatment as detected by comprehensive UHPLC HR TOF MS M. Sundström, A. Pelander, K. Simojoki and I. Ojanperä 8(1) (2016) ISSN

2 Reviews β Glucan is a valuable molecule molecule for the human and animal health system. The yeast cell wall, particularly of baker's and brewer's yeast Saccharomyces cerevisiae, is an important source of β D glucans. For yeast β glucan, many extraction methods have been proposed. Yeast cells can be exploited for β glucan production. Brewery and winery spent yeast biomass can comprise an alternative source for β glucan production. An evaluation study of different methods for the production of β D glucan from yeast biomass V. Varelas, M. Liouni, A. C. Calokerinos and E. T. Nerantzis Literature review suggests cannabinoid analysis as essential requirement to estimate the time of last cannabis intake supporting a temporal relationship between marijuana smoking and CVD. Any scientific interference about a causal link between cannabis use and CVD remains plausible but not completely established. Coronary thrombosis and marijuana smoking: a case report and narrative review of the literature D. Marchetti, A. Spagnolo, V. De Matteis, L. Filograna and N. De Giovanni During the three year period of we have found the new psychoactive substances (NPS) in 112 cases. The drugs detected were: 3 MMC, α PVP, MDPBP, UR 144, ethcathinone, mephedrone, MDPV, 4 MEC, buphedrone, 2 DPMP, methylone and 2C B. In single cases, 2 MMC, 2C P, eutylone, 25I NBOMe, mcpp, ephedrone, MPA and 5 APB were found. The prevalence of new psychoactive substances in biological material a threeyear review of casework in Poland P. Adamowicz, J. Gieroń, D. Gil, W. Lechowicz, A. Skulska and B. Tokarczyk 2

3 3 Pharmaceutical applications of NIR CI in each unit operation during the manufacturing processes, from the Western solid dosage forms to the Chinese materia medica preparations, are reviewed. PAT: From Western solid dosage forms to Chinese materia medica preparations using NIR CI L. Zhou, M. Xu, Z. Wu, X. Shi and Y. Qiao Research articles A method is developed and validated for simultaneous screening and quantification of 24 analytes of forensic relevance in vitreous humour, blood and plasma using LC MS/MS. The method is advantageous over other methods due to its simplified sample preparation protocol and less sample requirement. The method is well applied for screening of drugs in post mortem samples collected at autopsy. Development and validation of an ESI LC MS/ MS method for simultaneous identification and quantification of 24 analytes of forensic relevance in vitreous humour, whole blood and plasma B. Arora, T. Velpandian, R. Saxena, S. Lalwani, T. D. Dogra and S. Ghose 2 Methoxydiphenidine (2 MXP) has recently appeared as a research chemical and is suspected to show dissociative properties in humans. This study presents the identification of 2 MXP in various products obtained from test purchases from UK based vendors. Further verification was obtained by organic synthesis of three positional MXP isomers. Furthermore, the implementation of matrix assisted inlet ionization Orbitrap mass spectrometry confirmed the ability to detect the protonated molecule of 2 MXP directly from the tablet surface following addition of 3 nitrobenzonitrile as the matrix. Test purchase, synthesis, and characterization of 2 methoxydiphenidine (MXP) and differentiation from its meta and parasubstituted isomers G. McLaughlin, N. Morris, P. V. Kavanagh, J. D. Power, J. O'Brien, B. Talbot, S. P. Elliott, J. Wallach, K. Hoang, H. Morris and S. D. Brandt

4 The influence of several factors in the excretion of testosterone metabolites (Δ 1 AED, Δ 6 AED, Δ 6 T and Δ 15 AD) conjugated with cysteine is evaluated. These factors are divided into sample preservation (microbial degradation and freeze/thaw cycles), endogenous factors (gender, ultradian and circadian rhythms, pregnancy and UGT2B17 polymorphism), and exogenous factors (alcohol and 5α reductase inhibitors). The results show the stability of the urinary cysteinyl steroids under the influence of many factors, proving their potential as adequate parameters to be included in screening procedures applied in doping control. Factors affecting urinary excretion of testosterone metabolites conjugated with cysteine A. Fabregat, J. Marcos, J. Segura, R. Ventura and O. J. Pozo Short communications QTc shortening has been suggested as a method of screening for anabolic steriod abuse. This study evaluates the accuracy of such a test in a group of a long term steriod users. Prolonged androgenic anabolic steroid (AAS) induced QT interval shortening: a suitable screening tool? N. Sculthorpe, L. Taylor and F. M. Grace A new SPE HPLC MS method was developed to measure progestins and applied for the analysis of freshwater samples from Lake Balaton. HPLC MS/MS analysis of steroid hormones in environmental water samples P. Avar, G. Maasz, P. Takács, S. Lovas, Z. Zrinyi, R. Svigruha, A. Takátsy, L. G. Tóth and Z. Pirger 4

5 Handling cannabis plant material leads to a relevant and persistent contamination of hair with Δ 9 tetrahydrocannabinolic acid A (THCA A) and Δ 9 tetrahydrocannabinol (THC). Concentrations and pattern of distribution along the hair shaft are not distinguishable from typical results in hair samples of known cannabis users. In the light of the results of this study, any use of THC cut off concentrations in hair to evaluate consumption habits or frequency is strongly discouraged. Hair analysis for Δ9 tetrahydrocannabinolic acid A (THCA A) and Δ9 tetrahydrocannabinol (THC) after handling cannabis plant material B. Moosmann, N. Roth and V. Auwärter Correspondence case report Smoking habits of italian athletes undergoing anti doping control R. Pacifici, S. Pichini, I. Palmi, X. de la Torre and F. Botrè and the Anti-doping Commission at the Ministry of Health Application note The use of presumptive color tests for new psychoactive substances E. Cuypers, A.-J. Bonneure and J. Tytgat Research article Following intra articular administration to exercised Thoroughbred horses isoflupredone was detected for up to 36 and 48 h in plasma and urine, respectively. Furthermore, as isoflupredone was detected in synovial fluid for up to 14 days post administration, urine and blood concentrations do not appear to be good indicators of drug concentrations at the effector site and by and by extrapolation may not be useful in determining the duration of pharmacologic effect. Disposition of isoflupredone acetate in plasma, urine and synovial fluid following intra articular administration to exercised Thoroughbred horses H. K. Knych, L. M. Harrison, A. White and D. S. McKemie 5