Recent developments in the use of isotope ratio mass spectrometry in sports drug testing

Piper, Thomas; Emery, Caroline M.; Saugy, Martial

doi:10.1007/s00216-011-4886-6

Cited by 68 publications

(70 citation statements)

References 110 publications

(197 reference statements)

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“…Differences between the genders were not detected; this may be attributed to the fact that out of 29 investigated females, only seven used oral contraceptives, which are presumed to be responsible for gender-related differences [4,32].…”

Section: Factors Influencing Circontrasting

confidence: 54%

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Combination of carbon isotope ratio with hydrogen isotope ratio determinations in sports drug testing

et al. 2013

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Carbon isotope ratio (CIR) analysis has been routinely and successfully applied to doping control analysis for many years to uncover the misuse of endogenous steroids such as testosterone. Over the years, several challenges and limitations of this approach became apparent, e.g., the influence of inadequate chromatographic separation on CIR values or the emergence of steroid preparations comprising identical CIRs as endogenous steroids. While the latter has been addressed recently by the implementation of hydrogen isotope ratios (HIR), an improved sample preparation for CIR avoiding co-eluting compounds is presented herein together with newly established reference values of those endogenous steroids being relevant for doping controls. From the fraction of glucuronidated steroids 5β-pregnane-3α,20α-diol, 5α-androst-16-en-3α-ol, 3α-Hydroxy-5β-androstane-11,17-dione, 3α-hydroxy-5α-androstan-17-one (ANDRO), 3α-hydroxy-5β-androstan-17-one (ETIO), 3β-hydroxy-androst-5-en-17-one (DHEA), 5α- and 5β-androstane-3α,17β-diol (5aDIOL and 5bDIOL), 17β-hydroxy-androst-4-en-3-one and 17α-hydroxy-androst-4-en-3-one were included. In addition, sulfate conjugates of ANDRO, ETIO, DHEA, 3β-hydroxy-5α-androstan-17-one plus 17α- and androst-5-ene-3β,17β-diol were considered and analyzed after acidic solvolysis. The results obtained for the reference population encompassing n = 67 males and females confirmed earlier findings regarding factors influencing endogenous CIR. Variations in sample preparation influenced CIR measurements especially for 5aDIOL and 5bDIOL, the most valuable steroidal analytes for the detection of testosterone misuse. Earlier investigations on the HIR of the same reference population enabled the evaluation of combined measurements of CIR and HIR and its usefulness regarding both steroid metabolism studies and doping control analysis. The combination of both stable isotopes would allow for lower reference limits providing the same statistical power and certainty to distinguish between the endo- or exogenous origin of a urinary steroid.

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Section: Factors Influencing Circontrasting

confidence: 54%

“…Several factors influencing the CIR of endogenous steroids have been identified in previous studies [4][5][6]32]. Within the present study, a significant difference (t test, p<0.001) was detected only between steroids excreted glucuronidated or sulfoconjugated.…”

Section: Factors Influencing Cirsupporting

confidence: 35%

Combination of carbon isotope ratio with hydrogen isotope ratio determinations in sports drug testing

et al. 2013

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“…However, silylation introduces many foreign atoms and derivatized compounds have a limited storage lifetime. It is suspected that silicon carbide is formed in the reductive high-temperature conversion oven [115] leading to incomplete combustion [22,116]; this reduces precision [116] and precludes hydrogen isotope analysis [117].…”

Section: Silylationmentioning

confidence: 99%

Current challenges in compound-specific stable isotope analysis of environmental organic contaminants

et al. 2012

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Compound-specific stable-isotope analysis (CSIA) has greatly facilitated assessment of sources and transformation processes of organic pollutants. Multielement isotope analysis is one of the most promising applications of CSIA because it even enables distinction of different transformation pathways. This review introduces the essential features of continuous-flow isotope-ratio mass spectrometry (IRMS) and highlights current challenges in environmental analysis as exemplified for the isotopes of nitrogen, hydrogen, chlorine, and oxygen. Strategies and recent advances to enable isotopic measurements of polar contaminants, for example pesticides or pharmaceuticals, are discussed with special emphasis on possible solutions for analysis of low concentrations of contaminants in environmental matrices. Finally, we discuss different levels of calibration and referencing and point out the urgent need for compound-specific isotope standards for gas chromatography-isotope-ratio mass spectrometry (GC-IRMS) of organic pollutants.

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“…An invaluable addition to this strategy is the use of the isotope ratio mass spectrometry (IRMS). This technique allows to differentiate between natural and synthetic endogenous steroids by means of the ratios of the stable carbon isotopes 13 C and 12 C,38 39 that is, a suspicion of the misuse of endogenous AAS, triggered by the steroidal module of the ABP, can be proven by subsequent IRMS analyses.…”

Section: Introductionmentioning

confidence: 99%

Anabolic agents: recent strategies for their detection and protection from inadvertent doping

2014

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According to the World Anti-Doping Agency (WADA) Prohibited List, anabolic agents consist of exogenous anabolic androgenic steroids (AAS), endogenous AAS and other anabolic agents such as clenbuterol and selective androgen receptor modulators (SARMs). Currently employed strategies for their improved detection include the prolongation of the detection windows for exogenous AAS, non-targeted and indirect analytical approaches for the detection of modified steroids (designer steroids), the athlete’s biological passport and isotope ratio mass spectrometry for the detection of the misuse of endogenous AAS, as well as preventive doping research for the detection of SARMs. The recent use of these strategies led to 4–80-fold increases of adverse analytical findings for exogenous AAS, to the detection of the misuse of new designer steroids, to adverse analytical findings of different endogenous AAS and to the first adverse analytical findings of SARMs. The strategies of the antidoping research are not only focused on the development of methods to catch the cheating athlete but also to protect the clean athlete from inadvertent doping. Within the past few years several sources of inadvertent doping with anabolic agents have been identified. Among these are nutritional supplements adulterated with AAS, meat products contaminated with clenbuterol, mycotoxin (zearalenone) contamination leading to zeranol findings, and natural products containing endogenous AAS. The protection strategy consists of further investigations in case of reasonable suspicion of inadvertent doping, publication of the results, education of athletes and development of methods to differentiate between intentional and unintentional doping.

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Recent developments in the use of isotope ratio mass spectrometry in sports drug testing

Cited by 68 publications

References 110 publications

Combination of carbon isotope ratio with hydrogen isotope ratio determinations in sports drug testing

Combination of carbon isotope ratio with hydrogen isotope ratio determinations in sports drug testing

Current challenges in compound-specific stable isotope analysis of environmental organic contaminants

Anabolic agents: recent strategies for their detection and protection from inadvertent doping

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