Mass spectrometric identification and characterization of a new long-term metabolite of metandienone in human urine

Rapid Commun Mass Spectrom. 2006;20(15):2252-2258
Schanzer W, Geyer H, Fussholler G, Halatcheva N, Kohler M, Parr MK, Guddat S, Thomas A, Thevis M.
Center for Preventive Doping Research-Institute of Biochemistry, German Sport University Cologne, Carl-Diem Weg 6, 50933 Cologne, Germany.
PubMed ID & Record: 16804957

Anabolic-androgenic steroids are some of the most frequently detected drugs in amateur and professional sports. Doping control laboratories have developed numerous assays enabling the determination of administered drugs and/or their metabolic products that allow retrospectives with respect to pharmacokinetics and excretion profiles of steroids and their metabolites. A new metabolite generated from metandienone has been identified as 18-nor-17beta-hydroxymethyl,17alpha-methyl-androst-1,4,13-trien-3-one in excretion study urine samples providing a valuable tool for the long-term detection of metandienone abuse by athletes in sports drug testing. The metabolite was characterized using gas chromatography/(tandem) mass spectrometry, liquid chromatography/tandem mass spectrometry and liquid chromatography/high-resolution/high-accuracy (tandem) mass spectrometry by characteristic fragmentation patterns representing the intact 3-keto-1,4-diene structure in combination with typical product ions substantiating the proposed C/D-ring structure of the steroid metabolite. In addition, structure confirmation was obtained by the analysis of excretion study urine specimens obtained after administration of 17-CD(3)-labeled metandienone providing the deuterated analogue to the newly identified metabolite. 18-Nor-17beta-hydroxymethyl,17alpha-methyl-androst-1,4,13-trien-3-one was determined in metandienone administration study urine specimens up to 19 days after application of a single dose of 5 mg, hence providing an extended detection period compared with commonly employed strategies.

Method development for cortisol and cortisone by micellar liquid chromatography using SDS: application to urine samples of rugby players

J Chromatogr Sci. 2005 May-Jun;43(5):235-40.
Izquierdo-Hornillos R, Gonzalo-Lumbreras R, Santos-Montes A.
Departamento de Química Analítica, Facultad de Ciencias Químicas, Universidad Complutense, 28040 Madrid, Spain.
PubMed ID & Record: 15975241

The chromatographic behavior of cortisol and cortisone using a micellar medium of sodium dodecyl sulphate (SDS) as surfactant, a Hypersil C18 (150- x 3.2-mm i.d., 5 microm) column, a flow rate of 0.5 mL/min, and UV absorbance detection at 245 nm is described. The effect of several organic modifiers and the surfactant concentration on the separation is studied. A mobile phase of 18 mM SDS and 8.3% tetrahydrofuran allows for the separation of cortisol and cortisone up to baseline. These results are also achieved by applying a bivariant optimization method. The proposed method is sensitive, reproducible, and selective. In addition, it is less expensive than conventional high-performance liquid chromatography methods for cortisol and cortisone. The method is applied to the determination of cortisol and cortisone in urine samples of rugby players before and after stress for doping control purposes.

Comment in: Fenske M. J Chromatogr Sci. 2006 Oct;44(9):579; author reply 580

World anti-doping regulations for 2005: essential changes for athletes and physicians

Arch Orthop Trauma Surg. 2006 May;126(4):286-8. Epub 2005 Dec 6.
Pabinger C, Gruber G.
Department of Orthopedics, Medical University Graz, Auenbruggerplatz 5-7, 8036 Graz, Austria.
PubMed ID & Record: 16333634

The World Anti-Doping Code was renewed by an international sports organization committee prior to the Olympic Games in Athens in 2004. Up to now, most of the important international sports federations have accepted the code. Governments will soon follow and set the legislative milestones for the fight against doping. Surveillance and code-conversion are being done by national anti-doping organizations.In 2005, the structural organization and the content of the 2004 prohibited list have been modified: "substances and methods prohibited all times" (in and out of competition); "substances and methods prohibited in competition", "substances prohibited in particular sports", and "specified substances" are separately discussed. News regarding "specific substances", "whereabout-infos" and "therapeutic use exemptions" are outlined clearly.

Hyphenated mass spectrometric techniques-indispensable tools in clinical and forensic toxicology and in doping control

J Mass Spectrom. 2006 Nov;41(11):1399-413
Maurer HH.
Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, University of Saarland, D-66421 Homburg (Saar), Germany.
PubMed ID & Record: 17051522

Hyphenated mass spectrometric techniques, particularly gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/mass spectrometry (LC/MS), are indispensable tools in clinical and forensic toxicology and in doping control owing to their high sensitivity and specificity. They are used for screening, library-assisted identification and quantification of drugs, poisons and their metabolites, prerequisites for competent expertise in these fields. In addition, they allow the study of metabolism of new drugs or poisons as a basis for developing screening procedures in biological matrices, most notably in urine, or toxicological risk assessment. Concepts and procedures using GC/MS and LC/MS techniques in the areas of analytical toxicology and the role of mass spectral libraries are presented and discussed in this feature article. Finally, perspectives of their future position are discussed.

Doping in fitness sports: estimated number of unreported cases and individual probability of doping

Addiction. 2006 Nov;101(11):1640-4
Simon P, Striegel H, Aust F, Dietz K, Ulrich R.
University of Tuebingen, Department of Sports Medicine, General Internal Medicine V, Tuebingen, Germany.
PubMed ID & Record: 17034444

AIMS: Recent studies have suggested that the use of doping substances and particularly of anabolic androgenic steroids (AAS) is often practised by fitness centre visitors. These studies employed direct interview techniques and questionnaires to assess the estimated number of unreported cases of doping. Because people hesitate to provide compromising information about themselves, these techniques are subject to response errors. In this study we applied an alternative interview technique to assess more accurately unreported cases of doping in fitness centres. DESIGN AND PARTICIPANTS: The present investigation employed the randomized response technique (RRT) to reduce response errors. A cohort of 500 people from 49 fitness centres participated in this study. FINDING: The RRT revealed a high prevalence of doping (12.5%). In addition, and most importantly, the present RRT study revealed an alarmingly high prevalence of illicit drug use, specifically of cocaine use, that has been severely underestimated by previous studies. CONCLUSIONS: The RRT confirmed previously estimated rates of AAS use assessed by direct interview techniques and voluntary questionnaires, but uncovered a much higher usage rate of illicit drugs among fitness centre visitors. This outcome enabled us to construct a 'probability' rating for the use of doping substances in fitness centre visitors. Given its high prevalence and the predominant use of AAS, doping among fitness centre visitors is an issue of extreme relevance for the health care system. Our study may help to characterize further doping substance users and to develop and apply prevention and intervention programmes specifically to individuals at high risk.