In order to improve their performances, even professional sportsmen are often tempted to take dietary supplements, as is evidenced by a considerable number of surveys documenting the prevalence of supplement use among athletes. An important factor stimulating this widespread use of supplements is of course the easy availability of these products through numerous Internet sites. Unfortunately, the athletes who take supplements are often largely unaware of the risks involved in the intake of these so-called ‘natural’ supplements. It appears to be common for sportsmen to exceed the recommended dosages, even though some of these substances, such as iron and zinc, are known to be harmful in higher doses. Another significant risk related to the intake of dietary supplements is that these products might be contaminated with anabolic steroids and could therefore lead to athletes failing a doping test or cause health risks to consumers. In order to clarify the extent of the problem, a broad-based investigation of the international nutritional supplement market was conducted.
From October 2000 until November 2001, a total of 634 non-hormonal dietary supplements were obtained from 215 different suppliers in 13 countries. These supplements were analyzed by means of a targeted gas chromatography–mass spectrometry (GC–MS) method, screening for testosterone, nandrolone, boldenone and their respective prohormones. Out of these 643 supplements, 94 (14.6%) were found to contain one of these anabolic steroids and one or more of their respective prohormones, none of which were identified on the label. This study shows that the contamination of dietary supplements is indeed an internationally prevalent problem, warranting the need for adequate screening methods to detect these anabolic steroids. In this manner, the risks of both positive doping tests and potentially serious health problems in athletes who take large amounts of these supplements can be minimized.
The aim of the present study was to develop such a new in-house mass spectral library of 88 steroids, along with a fast ultra-performance liquid chromatography (UPLC)–MS method, as a potentially attractive alternative to GC–MS, accurate mass measurements and bioactivity screening. In order to highlight the possibilities and limits of these libraries, the method was also tested on a number of samples already analyzed by means of a targeted LC–MS/MS method.
Becue I, Poucke CV, Peteghem CV. An LC-MS screening method with library identification for the detection of steroidsin dietary supplements. J Mass Spectrom 2011;46(3):327-35. An LC-MS screening method with library identificat... [J Mass Spectrom. 2011] - PubMed result
For many years anabolic-androgenic steroids (AAS) are by far the most frequently detected pharmacological substances in doping control. In order to improve their performances, professional sportsmen are often tempted to take dietary supplements. However, due to the frequent and widespread occurrence of contaminated supplements, the use of such products is not without risk for the athletes involved. In order to minimize the chances of an unattended positive doping test or serious health problems, fast and reliable screening methods for the detection of anabolic steroids in dietary supplements are needed. A general screening procedure requires the fast and unambiguous detection of a large range of steroids. Gas chromatography-mass spectrometry (GC-MS) has been used intensively in the detection of doping substances for the past 40 years. Over time, many laboratories have delivered spectra to be included in standard reference databases, one of which is maintained by the National Institute of Standards and Technology (NIST) (Gaithersburg, MD, USA). In recent years, however, liquid chromatography coupled to mass spectrometry (LC-MS) has gained popularity. Unfortunately, existing GC-MS libraries are not applicable to LC-MS analysis. In the present study, a new mass spectral library of 88 steroids was developed, along with a fast UPLC-MS method. For the construction of this mass spectral library, three different mass spectra were measured for each steroid, with a sample cone voltage of 30, 60 and 100 V, respectively. This method was then successfully tested on contaminated dietary supplements which had previously been tested by means of a targeted LC-MS/MS method. Overall, the library search was shown to identify the same compounds as the MRM method.
From October 2000 until November 2001, a total of 634 non-hormonal dietary supplements were obtained from 215 different suppliers in 13 countries. These supplements were analyzed by means of a targeted gas chromatography–mass spectrometry (GC–MS) method, screening for testosterone, nandrolone, boldenone and their respective prohormones. Out of these 643 supplements, 94 (14.6%) were found to contain one of these anabolic steroids and one or more of their respective prohormones, none of which were identified on the label. This study shows that the contamination of dietary supplements is indeed an internationally prevalent problem, warranting the need for adequate screening methods to detect these anabolic steroids. In this manner, the risks of both positive doping tests and potentially serious health problems in athletes who take large amounts of these supplements can be minimized.
The aim of the present study was to develop such a new in-house mass spectral library of 88 steroids, along with a fast ultra-performance liquid chromatography (UPLC)–MS method, as a potentially attractive alternative to GC–MS, accurate mass measurements and bioactivity screening. In order to highlight the possibilities and limits of these libraries, the method was also tested on a number of samples already analyzed by means of a targeted LC–MS/MS method.
Becue I, Poucke CV, Peteghem CV. An LC-MS screening method with library identification for the detection of steroidsin dietary supplements. J Mass Spectrom 2011;46(3):327-35. An LC-MS screening method with library identificat... [J Mass Spectrom. 2011] - PubMed result
For many years anabolic-androgenic steroids (AAS) are by far the most frequently detected pharmacological substances in doping control. In order to improve their performances, professional sportsmen are often tempted to take dietary supplements. However, due to the frequent and widespread occurrence of contaminated supplements, the use of such products is not without risk for the athletes involved. In order to minimize the chances of an unattended positive doping test or serious health problems, fast and reliable screening methods for the detection of anabolic steroids in dietary supplements are needed. A general screening procedure requires the fast and unambiguous detection of a large range of steroids. Gas chromatography-mass spectrometry (GC-MS) has been used intensively in the detection of doping substances for the past 40 years. Over time, many laboratories have delivered spectra to be included in standard reference databases, one of which is maintained by the National Institute of Standards and Technology (NIST) (Gaithersburg, MD, USA). In recent years, however, liquid chromatography coupled to mass spectrometry (LC-MS) has gained popularity. Unfortunately, existing GC-MS libraries are not applicable to LC-MS analysis. In the present study, a new mass spectral library of 88 steroids was developed, along with a fast UPLC-MS method. For the construction of this mass spectral library, three different mass spectra were measured for each steroid, with a sample cone voltage of 30, 60 and 100 V, respectively. This method was then successfully tested on contaminated dietary supplements which had previously been tested by means of a targeted LC-MS/MS method. Overall, the library search was shown to identify the same compounds as the MRM method.