Spectroscopy Focus Current Role of LC-MS/MS in Sports Drug Testing
Chromatographic and Mass Spectrometric techniques have become an invaluable tool in the continuing fight against illegal doping in sport. The great majority of current assays employed in this field rely on the power of identification obtained from retention times and (product ion) mass spectra derived from hundreds of target analytes. The inventive nature of cheating athletes and the growing pool of drugs and therapeutics have necessitated the need for comprehensive, sensitive and specific detection methods and LC combined with MS has been shown to provide the necessary characteristic for the detection of low and high molecular weight compounds. Professor Mario Thevis here outlines the problems, challenges and successes in this continuing war against the cheats.
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Our laboratory is equipped with various different LC and MS systems, all of which provide characteristics that are particularly useful for our work.
Author Details:
Professor Dr Mario Thevis, German Sport University Cologne, Centre for Preventive Doping Research/Institute of Biochemistry, Cologne, Germany.
Bernie Monaghan (BM): Could you tell us a little about the group in which you work in Cologne and what are the aims and objectives of the group?
Mario Thevis (MT): I am working at the Institute of Biochemisty and Center for Preventive Doping Research at the German Sport University in Cologne. Besides routine doping controls (approx. 13,000 samples/year), we develop and establish new doping control strategies and methods to enable the identification of emerging drugs before these compounds enter the pharmaceutical market. This should reduce the window of opportunity that cheating athletes’ might have when abusing a new, probably not even approved drug.
BM: Which Instruments do you have available to allow you to meet these objectives? Are there particular technological reasons for one manufactures equipment, maybe sensitivity or interface characteristics which make your job easier?
MT: Our laboratory is equipped with various different LC and MS systems, all of which provide characteristics that are particularly useful for our work. The systems include regular (normal flow) liquid chromatography as well as micro- and nanoflow LC provided by Agilent, Thermo, and Waters. The mass spectrometers range from triple quadrupole, over quadrupole-linear ion trap, Orbitrap, to linear ion trap-Orbitrap systems to ensure robust target screening, quantitation, and allow general unknown analyses.
BM: Which were the first types of drugs that were successfully detected using the LC-MS/MS type of detection
MT: One of the first applications using LC- MS(/MS) in our laboratory was established concerning corticosteroids and those anabolic steroids that are hardly analysed by means of GC-MS due to thermal instability and formation of artefacts. The gain in sensitivity was enormous.
Figure 1. Agilent 1100 series HPLC coupled to Applied Biosystems API4000 Q Trap.
A little later, the issue of detecting peptide hormones in sports drug testing samples was addressed using modern LC-MS/MS systems, and we successfully established procedures to measure physiological levels of insulins and respective metabolites in plasma and urine. [1], see figure 3.
BM: ‘Designer Steroids’ were a type of drug that had a very high public profile and sounded very glamorous and almost ‘side effect free’. How did you go about designing assays for these? What are the side effects of these products on the human body?
Figure 2. Thermo Fisher Exactive MS and Accela LC with Advion Triversa Nanomate interface.
MT: Designer steroids have challenged the doping control community for several years, and most of them are hardly (if at all) clinically or pharmacologically tested; hence, undesired effects are likely and presumably very dangerous, but that did not stop athletes from taking these products.
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