Carbon isotope mass spectrometry in doping control

Sobolevskii, T. G.; Prasolov, Ilya; Rodchenkov, G. M.

doi:10.1134/s1061934810080113

Cited by 14 publications

(12 citation statements)

References 9 publications

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“…Sorting of all steroids in ascending order by their CIR results in a distinctive pattern. Direct comparison with recently published data [10,14] shows that different methods or different investigated populations result in non-conformities regarding the pattern of herein measured CIR. For example, TESTO was found more depleted than 5aDIOL in this study (Fig.…”

Section: Reference Population-based Valuesmentioning

confidence: 85%

“…The CIR found within this population mainly reflect the expected values for a European population [4,5,7,10,11,14]. The results are depicted in Fig.…”

Section: Reference Population-based Valuesmentioning

confidence: 85%

“…Within the last years, the number of investigations on carbon isotope ratios (CIR) of endogenous urinary steroids in the context of sports drug testing has considerably increased [1][2][3][4][5][6][7][8][9][10][11][12][13][14]. Regarding absolute values expressed as δ 13 C VPDB against the international standard Vienna Pee Dee Belemnite (VPDB) based on Eq.…”

Section: Introductionmentioning

confidence: 99%

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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: Reference Population-based Valuesmentioning

confidence: 85%

“…The CIR found within this population mainly reflect the expected values for a European population [4,5,7,10,11,14]. The results are depicted in Fig.…”

Section: Reference Population-based Valuesmentioning

confidence: 85%

Section: Introductionmentioning

confidence: 99%

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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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“…Previously a number of new synthetic drugs and its metabolites were described [5][6][7][8]. The development of new methods of non-targeted screening for toxicological purposes is still relevant.…”

Section: Furanoylfentanylmentioning

confidence: 99%

Identification of Furanoylfentanil and its Metabolites in Human Urine

Av¹,

Az²,

Oa³

et al. 2017

J Environ Anal Toxicol

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“…The unique 13 C signature of synthetic steroids is currently used to test athletes for doping with synthetic androgens [28] and to detect the treatment of cattle with synthetic estrogens. [29] Our results suggest that 13 C could also be used to discriminate endogenous from synthetic estrogens in animal waste, wastewater effluent, and natural waters.…”

Section: Wileyonlinelibrarycom/journal/rcmmentioning

confidence: 99%

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

Griffith¹

2013

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Steroidal estrogens are potent endocrine disrupting chemicals that are naturally excreted by vertebrates (e.g., humans and fish) and can enter natural waters through the discharge of treated and raw sewage. Because estrogens are detrimental to aquatic organisms at picomolar concentrations, many studies have measured so-called "free" estrogen concentrations in wastewater effluents, rivers, and lakes. Yet, to our knowledge, no studies have characterized the broader range of estrogens that includes free, conjugated, and halogenated forms.Conjugated estrogens are important because they can be easily converted to potent free forms by bacteria in wastewater treatment plants and receiving waters. And halogenated estrogens, produced during wastewater disinfection, are only slightly less potent than free estrogens but much more likely to bioaccumulate.We have developed a tandem mass spectrometry method that is capable of simultaneously quantifying free, conjugated, and halogenated estrogens at picomolar levels in wastewater effluent and coastal seawater. The method was validated using treated effluent from the greater Boston metropolitan area, where we found that halogenated estrogens represented over 50 % of the total estrogen discharge flux. A kinetic model of estrogen halogenation was used to predict the distribution of free and halogenated forms in wastewater effluent and suggested that chlorinated estrogens may be formed en route to the wastewater treatment plant.In the receiving waters of Massachusetts Bay, we detected a range of conjugated, free, and halogenated forms at concentrations that were well-predicted by dilution near the sewage outfall. Farther downstream, we found significantly higher estrone concentrations which points to large inputs of estrogens from sources other than sewage. 4Finally, we have used compound-specific measurements of 13 C and 14 C in commercial and pharmaceutical estrogen preparations to evaluate the potential for using carbon isotopes to distinguish between synthetic and endogenous steroids in wastewater and other environmental matrices. Our results show that synthetic estrogens and progestogens exhibit significantly depleted δ 13 C values (~ -30 ‰) compared to endogenous steroids (-16 ‰ to -26 ‰). This isotopic difference should make it possible to apportion synthetic and endogenous hormone sources in complex environments.

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Carbon isotope mass spectrometry in doping control

Cited by 14 publications

References 9 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

Identification of Furanoylfentanil and its Metabolites in Human Urine

Natural and synthetic estrogens in wastewater treatment plant effluent and the coastal ocean

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