Simultaneous detection of 93 anabolic androgenic steroids in dietary supplements using gas chromatography tandem mass spectrometry.

In recent years, anabolic androgenic steroids (AASs) have been frequently detected as undeclared ingredients in dietary supplements, where the adverse analytical findings (AAFs) were obtained from analysis of athletes' urine samples after ingestion. In our present study, a GC-MS/MS method for simultaneous detection of 93 anabolic steroids was developed. The chromatographic and mass spectrometric conditions were optimized, and selective reaction monitoring (SRM) mode was adopted to obtain the necessary sensitivity. The whole sample analysis process was completed within 23 min, and the limit of detection (LOD) was 0.5-4 ng.g-1 for solid samples and 0.1-0.8 ng.mL-1 for liquid samples. This method was verified according to World Anti-Doping Agency (WADA) regulations. In addition, the method was found to be specific, accurate. The developed method was then applied to a routine analysis of more than 300 liquid and solid dietary supplements, and one testosterone-positive sample was found. Three suspected drugs, (4-hydroxyandrostenedione, DHEA, and 6-Br androstenedione) were found in three dietary supplements obtained from the Internet through the pretreatment method of this study. This study provides a high-throughput method for screening and monitoring the ingredients of supplements and their subsequent harm to public health.

Influences of musk administration on the doping test.

Musk is widely used as a traditional drug in Asia for the treatment of stroke, tumour, and cardiopathy with an oral dosage of 0.03-0.1 g per day. Because of the potential anabolic effect, musk preparations have been included in the list of medical products containing prohibited substances employed for doping. The application of musk pod formulation was regarded as the reason of some adverse analytical findings in the 2011 FIFA Women's World Cup. In order to investigate the influence of musk administration on the doping test, we executed a chemical analysis and excretion study. The gas chromatography/mass spectrometry (GC-MS) analysis demonstrated the diversity of steroid concentrations in musk samples. Furthermore, the δ(13)C-values of steroids from wild deer musk showed more depleted than those of domestic deer musk by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) analysis. Because the steroids from some musk had δ(13)C-values in the range of naturally produced steroids in human body, the possible abuse of this kind of musk is very hard to be detected by isotope ratio mass spectrometry (IRMS) in doping control. Musk grains from wild and domestic deer were administrated for the excretion study respectively. Spot urine samples were collected from two male volunteers before and after 100 mg musk grains administration. The profiles and carbon isotope ratios of urinary steroids were determined by GC-MS and GC/C/IRMS. The ingestion of either wild or domestic deer musk did not lead to the adverse analytical finding of doping control in the single dosage of 100mg.