Rationale High‐resolution mass spectrometry (HRMS) has been demonstrated to be an alternative platform for quantitative analyses, identifying unknown compounds and gathering information the elucidation of chemical structures. This work describes a method detect 13 esters testosterone (T) 5 biomarkers in 0.1 mL human serum using gas chromatography (GC) coupled HRMS. Methods Analytes were extracted from after deproteinization liquid–liquid extraction. The trimethylsilyl derivatives analyzed...

Formestane (4‐hydroxy‐androstenedione) is an aromatase inhibitor prohibited in sports and included, since 2004, the list of substances updated yearly by World Anti‐Doping Agency (WADA). Since endogenous production formestane has been described, it mandatory for anti‐doping laboratories to use isotope ratio mass spectrometry (IRMS) establish exogenous origin before issuing adverse analytical finding. The described IRMS methods detection are time‐consuming, requiring usually two consecutive...

Abstract The detection of clostebol misuse in sports has been growing recently, especially Italy, due to the ample availability pharmaceutical formulations containing acetate (Trofodermin®) and use more sensitive instrumentation by antidoping laboratories. Most these cases have claimed be related a nonconscious drug or through contact with relatives teammates using it. We investigated, application well‐known currently used gas chromatographic mass spectrometric procedures, likelihood...

Rationale Isotope ratio mass spectrometry (IRMS) is an analytical technique required by the World Antidoping Agency (WADA) before releasing of adverse finding for abuse pseudoendogenous steroids (i.e. testosterone). For every single individual, delta 13 C values (‰) selected target compounds (TCs, i.e. testosterone and/or its precursors/metabolites) are compared with those endogenous reference (ERCs). The aim this work to investigate individual variation in four different commonly used ERCs...

The detection of the abuse pseudo-endogenous steroids (testosterone and/or its precursors) is currently based on application steroid module World Anti-Doping Agency (WADA) Athletes' Biological Passport (ABP), implemented through ADAMS. Diagnostic metabolites are monitored for every athlete and statistically evaluated with a predictive Bayesian approach. In case suspicious samples, data ABP confirmed isotope ratio mass spectrometry (IRMS) test activated. We have previously demonstrated that...

The detection of testosterone and its precursors' abuse in antidoping sports analysis is based on the longitudinal evaluation markers urinary endogenous steroid profile. A Bayesian statistical approach applied, allowing establishment credible intervals selected parameters for every athlete. Samples showing values outside acceptable boundaries are additional confirmation by isotope ratio mass spectrometric (IRMS) analysis. alterations IRMS last longer than Then application to a larger number...

Abstract During the ozonation of triglycerides and unsaturated fatty acids from sunflower oil, aldehydes carboxylic with three, six nine carbon atoms are obtained, together hydroperoxides, ozonides other peroxide species. Some them present relatively low boiling points, constituting volatile fraction ozonized oil (OLEOZON®). In work, was characterized by Gas Chromatography - Mass Spectrometry (GC/MS) (GC) combined three different extraction techniques: gaseous purge cold trap collection,...

This work demonstrates the high potential of combining high-resolution mass spectrometry with chemometric tools, using metabolomics as a guided tool for anti-doping analysis. The administration 7-keto-DHEA was studied proof-of-concept effectiveness combination knowledge-based and machine-learning approaches to differentiate changes due athletic activities from those recourse doping substances methods.Urine samples were collected five healthy volunteers before after an oral by identifying...

Isoflavones are a group of flavonoids that may be interest in sport doping because they can used by athletes the recovery periods after administration anabolic steroids, with aim increasing natural production luteinizing hormone (LH) and, consequently, biosynthesis endogenous androgens.The vivo metabolism methoxyisoflavone (5-methyl-7-methoxyisoflavone) and ipriflavone (7-isopropoxyisoflavone), respectively present dietary supplement pharmaceutical preparation, was investigated. The study...

Systematic electron ionization fragmentation studies of steroids have been performed to elucidate and trace their characteristic patterns. However, the source setting at 70 eV energy is much higher than potential (7-15 eV) most organic compounds, leading extensive fragmentation. We present a multifactorial study on optimizing low-energy maximize molecular ion formation while minimizing extent improve analytical sensitivity steroids, especially more thermolabile ones, preserving information...

ABSTRACT This work aims to characterize the serum profile of athletes after administration ecdysteroids, natural steroid hormones recently reported enhance athletic performance. The combination mass spectrometry and chemometric tools may allow differentiate physiological effects from post‐training intake‐driven effects. Serum samples were collected 46 healthy male volunteers divided into four groups: control (two capsules/day Peak Ecdysone without training), placebo capsules ecdysteroids...