Development and Validation of an UHPLC–MS/MS Method for Extended Serum Steroid Profiling in Female Populations

Salamin, Olivier; Ponzetto, Federico; Cauderay, Michel Jean; Bernard, Julien; Saugy, Martial; Kuuranne, Tiia; Nicoli, Raul

doi:10.4155/bio-2020-0046

Cited by 21 publications

(16 citation statements)

References 30 publications

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“…The knowledge on how urine and serum androgen metabolites are connected may be of interest in anti-doping since quantification of endogenous serum steroids may be a complementary approach to the urinary steroid profile method in the future (Salamin et al, 2020). The monitoring of serum T may increase the likelihood to detect T intake in female athletes as serum T is superior compared to the urinary steroid profile (Handelsman and Bermon, 2019;Börjesson et al, 2020;Knutsson et al, 2020).…”

Section: Discussionmentioning

confidence: 99%

“…It has been shown that after 10 weeks of transdermal T application in healthy women, only 40% were identified as having atypical passport findings (Knutsson et al, 2020) even though their serum T levels were elevated to concentrations associated with performance enhancing effects (Hirschberg et al, 2020). As a supplementary method, the serum concentration of T, androstenedione and dihydrotestosterone may be co-monitored (Salamin et al, 2020) and subsequently there is an interest to understand the relation between the serum steroid concentrations and urinary excretion rate of the ABP metabolites.…”

Section: Introductionmentioning

confidence: 99%

“…We, and others, have previously shown that implementation of the ABP increases the chance to detect testosterone intake in men as compared to traditional population based cut-off values after administration of low dose of testosterone ( Strahm et al, 2015 ; Mullen J. et al, 2017 ; Nair et al, 2020 ). Furthermore, in women the longitudinal ABP approach is superior to the population-based thresholds to detect administered T, however, not all women are identified as having atypical findings ( Handelsman and Bermon, 2019 ; Knutsson et al, 2020 ; Salamin et al, 2020 ). It has been shown that after 10 weeks of transdermal T application in healthy women, only 40% were identified as having atypical passport findings ( Knutsson et al, 2020 ) even though their serum T levels were elevated to concentrations associated with performance enhancing effects ( Hirschberg et al, 2020 ).…”

Section: Introductionmentioning

confidence: 99%

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Urinary Steroid Profile in Elite Female Athletes in Relation to Serum Androgens and in Comparison With Untrained Controls

et al. 2021

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IntroductionIn female athletes, the interpretation of doping tests is complex due to hormonal variations during the menstrual cycle and hormonal contraceptive use, both influencing the urinary steroid profile. Exercise is suggested to affect circulating steroid hormone levels, and in women, the urinary steroid profile differs between in competition testing and out of competition testing. No previous study has investigated the relationship between amount of exercise and the urinary steroid profile in female elite athletes.PurposeTo compare the urinary steroid profile between female Olympic athletes and age- and BMI-matched untrained controls, and to study the urinary steroid profile in relation to serum hormones and amount of exercise.MethodsIn this cross-sectional study conducted at the Women’s Health Research Unit, Karolinska University Hospital, Stockholm, 94 female elite athletes and 86 untrained controls were included. Serum estrogens and testosterone and the urinary steroid profile were analyzed by liquid chromatography–tandem mass spectrometry and gas chromatography-tandem mass spectrometry, respectively. Exercise hours/week were evaluated by questionnaire.ResultsAlthough serum steroid hormones were comparable between groups, the athletes demonstrated approximately 30% lower urinary steroid metabolites of testosterone, epitestosterone, androsterone, etiocholanolone, 5α-androstan-3α, 17β-diol, and 5β-androstan-3α, 17β-diol compared to the controls. The urinary steroid metabolites correlated positively with serum steroid hormones. In the athletes, urinary steroid metabolites: androsterone (rs = −0.28, p = 0.007), epitestosterone (rs = −0.22, p = 0.034), 5αAdiol (rs = −0.31, p = 0.002) and testosterone (rs = −0.24, p = 0.026), were negatively correlated with amount of training (hours per week).ConclusionThe urinary concentrations of steroid metabolites were lower in elite athletes than in sedentary controls, although serum steroids were comparable between groups. Moreover, exercise time was negatively associated with the urinary concentrations. Our findings suggest alternative excretion routes of androgens in the athletes related to training.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Urinary Steroid Profile in Elite Female Athletes in Relation to Serum Androgens and in Comparison With Untrained Controls

et al. 2021

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“…Extending steroid profile analysis from urine to serum has been shown to be a promising complementary tool in anti‐doping analysis, and two analytical assays were reported that allow for quantifying the most relevant conjugated and unconjugated androgens. Salamin et al employed SPE to extract steroidal analytes from acidified serum, followed by concentration of the extract and subsequent LC‐MS/MS analysis 78 . Fourteen unconjugated steroids as well as 7 sulfo‐ and 7 glucurono‐conjugates were separated on a C‐18 analytical column (150 × 2.1 mm, 1.7 μm particle size) with 5‐mM ammonium formate (mobile phase A) and methanol (containing 5‐mM ammonium formate, mobile phase B), with T, EpiT, A, E, and EpiA being monitored as sulfates and glucuronides, while 5βAdiol was included as 3‐ and 17‐ O ‐glucuronide only and DHEA and norE as sulfate only.…”

Section: Anabolic Agentsmentioning

confidence: 99%

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Thevis

Kuuranne

Geyer

2020

Drug Testing and Analysis

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Analytical chemistry-based research in sports drug testing has been a dynamic endeavor for several decades, with technology-driven innovations continuously contributing to significant improvements in various regards including analytical sensitivity, comprehensiveness of target analytes, differentiation of natural/ endogenous substances from structurally identical but synthetically derived compounds, assessment of alternative matrices for doping control purposes, and so forth. The resulting breadth of tools being investigated and developed by anti-doping researchers has allowed to substantially improve anti-doping programs and data interpretation in general. Additionally, these outcomes have been an extremely valuable pledge for routine doping controls during the unprecedented global health crisis that severely affected established sports drug testing strategies. In this edition of the annual banned-substance review, literature on recent developments in antidoping published between October 2019 and September 2020 is summarized and discussed, particularly focusing on human doping controls and potential applications of new testing strategies to substances and methods of doping specified the World Anti-Doping Agency's 2020 Prohibited List.

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“…Finally, the work of Nicoli and colleagues confirms that ultra high-performance LC (UHPLC)-tandem MS can provide reliable measurements of free and conjugated steroid concentrations in blood serum to complement those obtained by GC-MS/MS on free steroids in urine for the determination of the steroid profile required by WADA for the athlete biological passport. Furthermore, they illustrate the application of the method in the evaluation of females with mild hyperandrogenism and a group with normal circulating androgen levels, and suggest the clinical value of such an investigation as well as helping distinguish physiological outliers from sports cheats [11].…”

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confidence: 98%

Antidoping Analysis: A Special Focus

Cowan

2020

Bioanalysis

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in antidoping • gene doping • metabolomics in antidoping • peptide quantification • VAMS in antidopingThis issue of Bioanalysis has the theme of antidoping analysis and was originally planned to be published to coincide with the run-up to the 2020 Olympic and Paralympic Games in Tokyo, Japan. It was intended to give the interested reader an indication of the latest approaches used by the scientists working in the antidoping field that would likely be used during the Games in the Tokyo World Anti-Doping Agency (WADA) accredited antidoping laboratory. The COVID-19 pandemic has affected all walks of life internationally and sport is no exception; hence the games have been postponed for a year until 2021 by the International Olympic Committee, for the first time ever. The ability, under WADA and International Olympic Committee regulations, to store samples for up to 10 years means that even if some of the approaches described in this issue are not yet ready for use to take action against a cheating athlete, retrospective analysis could enable this to occur at some time in the years ahead.I have found the articles in this issue always interesting to read and informative, being written by and with the opinions of experts in the field of antidoping science. The conclusions or opinions documented should provide fertile ground for further research. Here is a summary of what you will find.Aikin and colleagues from WADA provide a well-informed perspective about the current and future use of biomarkers in antidoping testing with a special focus on athlete biological passports pioneered by their organization. They outline what is required and make it clear that discovering new biomarkers and implementing their use is no easy task, but worth the effort in making antidoping testing more effective [1].Botré and colleagues provide a commentary on the need for a metabolomics approach to deal with some of the more complex analytical challenges in antidoping, and the potential of the approach for use in the field. However, they point out numerous challenges and conclude that "stand-alone screening + confirmation techniques based on metabolomics approaches still seem premature in antidoping," but indicate that explorative metabolomics are of value even now to help identify putative biomarkers [2].An update on the state of play of peptide quantification in antidoping and how it often links with the requirements of clinical science is provided in an editorial by Moncrieffe. The need for traceable reference standards is stressed and the importance of LC-MS to provide the 'gold-standard' approach contrasting with some of the problems encountered with the use of immuno-procedures. She stresses the benefits of and need for good interlaboratory studies to show the reliability and robustness of the methods [3].Fedoruk of the United States Anti-Doping Agency (USADA) presents in his editorial how USADA has modified its approach to antidoping testing as a result of the COVID-19 pandemic [4]. He explains how athletes attempt to beat the testers ...

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Development and Validation of an UHPLC–MS/MS Method for Extended Serum Steroid Profiling in Female Populations

Cited by 21 publications

References 30 publications

Urinary Steroid Profile in Elite Female Athletes in Relation to Serum Androgens and in Comparison With Untrained Controls

Urinary Steroid Profile in Elite Female Athletes in Relation to Serum Androgens and in Comparison With Untrained Controls

Annual banned‐substance review: Analytical approaches in human sports drug testing 2019/2020

Antidoping Analysis: A Special Focus

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