Urinary excretion profile of higenamine in females after oral administration of supplements - Doping scenario.

In 2017, higenamine was added to the World Antidoping Agency's (WADA) Prohibited list under group S3: beta-2 agonists and it is banned for athletes both in - and out of competition. Aim of this study was to characterize the urinary excretion profile of higenamine and its metabolite coclaurine after oral administration of multiple doses of higenamine capsules. For this purpose, an administration study including female basketball players was performed. For the detection of higenamine and cocalurine in the collected urine samples, a new, fast, and highly sensitive quantitative on-line SPE LC HRMS method was developed and validated. The method was applied for the quantification of higenamine and cocalurine in urine and their excretion pattern was defined. Results obtained show substantial inter-individual differences in the excretion profile of higenamine and coclaurine. For higenamine, half-lives were estimated to be between 4 and 27 h, and for coclaurine between 5 and 25 h. Furthermore, the data indicate that the elimination of coclaurine is rate-limited by its formation. Higenamine could be detected at a urine concentration above 10 ng/mL for at least 20 h after the last application for all study participants.

The uefa euro 2012 anti-doping programme - scientific review.

The final tournament of the UEFA European Football Championship is one of the top sporting events in the world, and a high-profile event of this kind requires a well-planned and well-executed anti-doping programme to ensure the integrity of results in the competition. UEFA EURO 2012 presented a unique logistical challenge, with the tournament spread across two countries, both covering a large geographical area. This paper discusses the planning and delivery of both the pre tournament out-of-competition (OOC) testing programme and the in-competition (IC) programme, as well as reviewing the activities of doping control officers (DCOs), the whereabouts programme and assessing the sample collection and transport process. The analytical approach applied is also discussed, along with an overview of the distribution of T/E ratios and blood parameters.

Screening of testosterone esters in human plasma.

The detection of an intact ester of testosterone in plasma is leading towards unequivocal proof of the administration of exogenous testosterone. In the current study, a sensitive screening method for the detection of nine testosterone esters in human plasma was developed. By preparing oxime derivatives of intact testosterone esters, the sensitivity of the assay was increased. Furthermore, the method included liquid-liquid extraction (LLE) as sample clean-up, as well as online separation of the target analytes from the derivatization solution. The analysis was performed by liquid chromatography (LC) coupled to tandem mass spectrometry (MS/MS). The method developed herein is simple and rapid, and was validated according to World Anti-Doping Agency (WADA) guidelines.

GASepo-a software solution for quantitative analysis of digital images in Epo doping control.

A software has been developed that is aimed at quantitative analysis of images acquired by isoelectric focusing and double blotting procedures used for recombinant erythropoietin doping control. It represents a unified and easy-to-use tool for Epo doping experts in WADA accredited laboratories. It is based on image segmentation philosophy that enables identification of individual bands whose characteristics are needed for evaluation of the Epo doping positivity criteria. Several modules implemented in the GASepo software include an original know how, in particular, the method of robust calculation of the cut-off line, band segmentation and classification algorithms. GASepo is being used in several doping control laboratories worldwide.

Quantitative analysis of images in erythropoietin doping control.

The software system GASepo has been developed as a tool to visualise and analyse doping (searching for performance-enhancing drugs in sports) with recombinant erythropoietin (rEpo). Digital images derived from the separation of Epo isoforms in gels by iso-electric focusing followed by double blotting and chemiluminescence detection contain spots (bands) of characteristic shape and positions. For Epo doping control, these have to be analysed and evaluated. A relevant element of the analysis is calculation of the reference cutoff-line (COL) to which the doping positivity criterion is related. Based on analysis of the previous method used, a novel method for the COL calculation was developed and validated. The methodology was based on generation of a partition of the image (lane) being processed into a system of adjacent subimages (blocks) and quantitative characterisation of intensity variability within these blocks by a suitably defined measure. The coordinate of the proper COL position, separating the image part with recombinant Epo bands from the homogeneous background, was calculated by minimisation of the difference function of the measures for two adjacent image blocks. The proposed method was tested on real Epo images and validated on a synthetic phantom of the Epo image. The deviations of the COL position are limited by a 7 pixel-wide corridor. For the cases of noise with standard deviations 2300 and 2600, the deviations did not exceed 2 pixels over the whole range of the lane width values. Testing the method on 50 real Epo images originating from different doping-control laboratories worldwide showed its robust behaviour in Epo images.

Quantification of ephedrines in urine by column-switching high-performance liquid chromatography.

A method for the quantification of five congener ephedrines in urine samples without sample preparation was developed. The analytes were trapped on a C18 precolumn and separated on a C18 BDS analytical column. Baseline separation was achieved for all analytes. The method meets the requirements of the International Olympic Committee (IOC) medical commission regarding cut-off limits for positive doping cases with ephedrines.

[Partner interactions and coping activity of migraine patients]. / Partnerschaftliches Interaktionsverhalten und Stressverarbeitung von Migränepatientinnen.

Empirical studies suggest that an inefficient, negative communication could represent a source of stress in the patient's everyday life and that this kind of communication would also imply chronic migraine. The present study used the "Kategoriensystem für partnerschaftliche Interaktion (KPI)" to determine whether the communication patterns of 12 women with migraine and their partners differed from 12 women with chronic headache and their partners and 12 healthy couples. The communication was video-filmed during the about 10 min lasting interaction in a personally relevant conflict situation. As predicted, women with migraine and their partners made more negative and fewer positive statements than the couples with tension headache and the control dyads. Furthermore, a higher load in female migraine sufferers compared to normal controls was indicated by coping activity.

Fast screening method for the profile analysis of polycyclic aromatic hydrocarbon metabolites in urine using derivatisation--solid-phase microextraction.

A method for the qualitative analysis of various metabolites of naphthalene, phenanthrene and pyrene is presented. The method uses SPME with a 85-microm polyacrylate fibre for extraction, headspace silylation with BSTFA without any catalyst for on-fibre derivatisation and GC-MS in the SIR mode for separation and detection. The suitability of the method for profile analysis of PAH metabolites is shown by analysing a smokers urine after enzymatic cleavage (and additionally after spiking with the target analytes) and spiked water. The method exhibits satisfactory separation of all investigated metabolites and no interferences due to matrix peaks.