Nutritional supplements cross-contaminated and faked with doping substances

Center for Preventive Doping Research, German Sport University Cologne, Am Sportpark Müngersdorf 6, 50933 Cologne, Germany.
Journal of Mass Spectrometry (Impact Factor: 2.38). 07/2008; 43(7):892-902. DOI: 10.1002/jms.1452
Source: PubMed


Since 1999 several groups have analyzed nutritional supplements with mass spectrometric methods (GC/MS, LC/MS/MS) for contaminations and adulterations with doping substances.
These investigations showed that nutritional supplements contained prohibited stimulants as ephedrines, caffeine, methylenedioxymetamphetamie and sibutramine, which were not declared on the labels. An international study performed in 2001 and 2002 on 634 nutritional supplements that were purchased in 13 different countries showed that about 15% of the nonhormonal nutritional supplements were contaminated with anabolic-androgenic steroids (mainly prohormones). Since 2002, also products intentionally faked with high amounts of ‘classic’ anabolic steroids such as metandienone, stanozolol, boldenone, dehydrochloromethyl-testosterone, oxandrolone etc. have been detected on the nutritional supplement market. These anabolic steroids were not declared on the labels either. The sources of these anabolic steroids are probably Chinese pharmaceutical companies, which sell bulk material of anabolic steroids. In 2005 vitamin C, multivitamin and magnesium tablets were confiscated, which contained cross-contaminations of stanozolol and metandienone. Since 2002 new ‘designer’ steroids such as prostanozol, methasterone, androstatrienedione etc. have been offered on the nutritional supplement market. In the near future also cross-contaminations with these steroids are expected. Recently a nutritional supplement for weight loss was found to contain the β2-agonist clenbuterol. The application of such nutritional supplements is connected with a high risk of inadvertent doping cases and a health risk. For the detection of new ‘designer’ steroids in nutritional supplements, mass spectrometric strategies (GC/MS, LC/MS/MS) are presented. Copyright

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    • "Additionally, some studies (Sousa et al., 2013; PetróCzi et al., 2007) have been denoting that athletes' choices are probably not based on scientific evidence. Moreover, the possible contamination of NS with prohibited substances in sport, which can result in inadvertent doping and health issues, is a current matter of high concern (Geyer et al., 2008). Some characteristics have previously been linked to NS usage, namely, the type of sport (Froiland et al., 2004), age (Erdman et al., 2007), and level of competition (Erdman et al., 2006). "
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    ABSTRACT: Purpose – The purpose of this paper is to analyse differences in sociodemographic and sporting characteristics, health-behaviours, and food intake of athletes using and not using nutritional supplements (NS). Design/methodology/approach – High-performance Portuguese athletes from 13 sports completed a NS usage questionnaire, assessing information on sociodemographic (sex, age, height, weight, athlete’s, and parental education level), health-related (smoking, daily time of sleeping, walking, and sitting), and sporting (type, number of international performances, weekly hours of training and weekly hours of gym) characteristics; and a semi-quantitative food-frequency questionnaire (86 items), regarding the previous 12 months. Findings – From the 241 athletes (66 per cent males, 13-37 years), 64 per cent reported NS use. Supplement usage was associated with age 18 years (odds ratio (OR) 2.57, 95 per cent; confidence interval (CI) 1.17-5.65), performing individual sports (OR 5.45, 95 per cent; CI 2.49-11.93) and >2 h gym/week (OR 2.42, 95 per cent; CI 1.15-5.11), a higher consumption of meat (OR 2.83, 95 per cent; CI 1.36-5.90), eggs (OR 2.53, 95 per cent; CI 1.07-5.96), and yogurt (OR 2.24, 95 per cent; CI 1.08-4.62), and a lower intake of processed meat (OR 0.32, 95 per cent; CI 0.15-0.72), vegetable oils (OR 0.35, 95 per cent; CI 0.17-0.74), margarine (OR 0.37, 95 per cent; CI 0.18-0.76), chips (OR 0.22, 95 per cent; CI 0.10-0.48), and fast food (OR 0.42, 95 per cent; CI 0.19-0.91). Originality/value – Athletes using NS had different characteristics from non-users, and seemed to have healthier and more sports-oriented food choices. Our findings may help sport and health professionals to identify an alleged or future NS user, enabling the development of a timely and self-directed supplement scheme.
    No preview · Article · Jan 2016 · British Food Journal
    • "Analytical methods for the determination of these doping agents in supplements include GC–MS, LC–MS/MS and HPLC-DAD in the case of anabolic agents [14] [15] [20] "
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    ABSTRACT: The quantitative analysis of a new designer doping agent, 2-ethylamino-1-phenylbutane (EAPB) and its metabolite, 2-amino-1-phenylbutane (APB) in urine samples, and the determination of EAPB in dietary supplement samples, have been presented. The main purpose of the present study was to develop simple and reliable gas chromatography-mass spectrometry method (GC-MS) for excretion study following a single oral administration of dietary supplements containing EAPB. Three analytical methods for the determination of EAPB in urine and supplement samples, and APB in urine samples using the GC-MS system, have been validated. The method of the determination of EAPB in supplement samples was applied to analyze seventeen dietary supplements, CRAZE and DETONATE. Two other methods were used to determine the urinary excretion profile of EAPB and APB in the case of three healthy volunteers and, on further investigation, it was applied to the anti-doping control in sport. Quantification was obtained on the basis of the ions at m/z 86, 58 and 169, monitored for EAPB, APB and diphenylamine (used as an internal standard), respectively. The limits of detection and quantification were 2.4 and 7.3μg/g for EAPB in the case of supplement analysis, 2.9 and 8.8ng/mL for EAPB in the case of urine analysis, and 3.2 and 9.7ng/mL for APB. The other validation parameters as linearity, precision and trueness have been also investigated with the acceptable results. The extraction yield of all presented methods was above 69%. EAPB was detected in fourteen analyzed supplements (not included EAPB in their labels) and its content varied between 1.8 and 16.1mg/g. Following oral administration of three supplements with EAPB to one male and two female volunteers, the parent compound of EAPB and its metabolite were monitored and the excretion parameters as the maximum concentration of the analyte in urine (2.2-4.2μg/mL for EAPB; 1.1-5.1μg/mL for APB) and the time for the maximum height of the excretion peak (2-8h and 22h in one case for EAPB; 20-22h and 4h in one case for APB) have been indicated. EAPB and APB were detected at the level above 50ng/mL (50% of the minimum required performance level for stimulants in the anti-doping control in-competition in sport) in the urine up to 46-106h and 58-120h, respectively. Additionally, the result of the anti-doping control during swimming competition of one athlete, whose urine sample was analyzed for stimulants and narcotics, has been presented. The qualitative and quantitative analyses of new designer agents in urine samples and the excretion studies of these substances are of a great importance in the anti-doping control in sport. Moreover, the presentation of detection examples of these agents in supplements that haven't got included an information about them in the labeling, make athletes (and other supplement customers) more and more aware of the risk of the supplement use and possible health and doping consequences. Copyright © 2015 Elsevier B.V. All rights reserved.
    No preview · Article · Jul 2015 · Journal of pharmaceutical and biomedical analysis
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    • "This specific sample is presented as a product manufactured by British Dispensary in Thailand and is known to have been falsified and marketed all over the world. [3] The main analytical techniques currently implemented to analyze these products are well described in the literature and include liquid chromatography with UV detection, [12] [15] [16] liquid chromatography with tandem mass detection, [4] [6] [13] [15] gas chromatography with mass detection [4,8,11–15] and sometimes nuclear magnetic resonance (NMR). [7] These methods are highly specific for the identification of anabolic steroid compounds and provide quantitative information but they involve destructive sample preparation. "
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    ABSTRACT: The use of performance enhancing drugs is a widespread phenomenon in professional and leisure sports. A spectroscopic study was carried out on anabolic tablets labelled as 5 mg methandienone tablets provided by police departments. The analytical approach was based on a two-step methodology: a fast analysis of tablets using near infrared (NIR) spectroscopy to assess sample homogeneity based on their global composition, followed by Raman chemical imaging of one sample per NIR profile to obtain information on sample formulation. NIR spectroscopy assisted by a principal components analysis (PCA) enabled fast discrimination of different profiles based on the excipient formulation. Raman hyperspectral imaging and multivariate curve resolution - alternating least square (MCR-ALS) provided chemical images of the distribution of the active substance and excipients within tablets and facilitated identification of the active compounds. The combination of NIR spectroscopy and Raman chemical imaging highlighted dose-to-dose variations and succeeded in the discrimination of four different formulations out of eight similar samples of anabolic tablets. Some samples contained either methandienone or methyltestosterone whereas one sample did not contain an active substance. Other ingredients were sucrose, lactose, starch or talc. Both techniques were fast and non-destructive and therefore can be carried out as exploratory methods prior to destructive screening methods. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.
    Full-text · Article · Jul 2015 · Drug Testing and Analysis
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