Determination of the Origin of 19-Norandrosterone in Urine by Gas Chromatography–Isotope-Ratio Mass Spectrometry for Doping Control

Podolskiy, Ilya; Sobolevskii, T. G.; Dikunets, M. A.

doi:10.1134/s1061934818010082

Cited by 4 publications

(4 citation statements)

References 12 publications

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“…They are included as anabolic androgenic steroids (AAS) in Section S1.1 of the Prohibited List written and regularly updated by the World Anti-Doping Agency (WADA). 29 In doping analysis, the detection of 19-norsteroids is currently performed through a gas chromatographytandem mass spectrometry (GC-MS/MS) semiquantitative determination of their major metabolite 19-NA, typically produced about three times more than 19-NE, 30,31 even if different excretion ratios have been also determined. 32 19-NA and 19-NE could be found at low concentrations in urine even if no exogenous and intentional administration of nandrolone or its precursors occurred.…”

Section: Introductionmentioning

confidence: 99%

“…Adequate strategies have been adopted in some WADA Accredited Antidoping Laboratories to determine the origin of 19-norsteroids metabolites. 31,52,53 A fast and simplified GC-C-IRMS procedure on underivatized 19-NA has been effectively set up and routinely applied in our laboratory. 54 In case of IRMS results inconclusive or consistent with endogenous values, the 19-NA/19-NE ratio is determined to confirm or not the atypical results to the antidoping test.…”

Section: Introductionmentioning

confidence: 99%

“…The IRMS analysis allows the discrimination between the exogenous or endogenous origin of steroid compounds, by exploiting their different 13 C content (expressed as δ 13 C [‰]). Adequate strategies have been adopted in some WADA Accredited Antidoping Laboratories to determine the origin of 19‐norsteroids metabolites 31,52,53 . A fast and simplified GC‐C‐IRMS procedure on underivatized 19‐NA has been effectively set up and routinely applied in our laboratory 54 .…”

Section: Introductionmentioning

confidence: 99%

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Detecting the abuse of 19‐norsteroids in doping controls: A new gas chromatography coupled to isotope ratio mass spectrometry method for the analysis of 19‐norandrosterone and 19‐noretiocholanolone

Iannella

Colamonici

Curcio

et al. 2020

Drug Testing and Analysis

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The detection of 19-norsteroids abuse in doping controls currently relies on the determination of 19-norandrosterone (19-NA) by gas chromatography-tandem mass spectrometry (GC-MS/MS). An additional confirmatory analysis by gas chromatography coupled to isotope ratio mass spectrometry (GC-C-IRMS) is performed on samples showing 19-NA concentrations between 2.5 and 15 ng/ml and not originated from pregnant female athletes or female treated with 19-norethisterone.19-Noretiocholanolone (19-NE) is typically produced to a lesser extent as a secondary metabolite. The aim of this work was to improve the GC-C-IRMS confirmation procedure for the detection of 19-norsteroids misuse. Both 19-NA and 19-NE were analyzed as target compounds (TCs), whereas androsterone (A), pregnanediol (PD), and pregnanetriol (PT) were selected as endogenous reference compounds (ERCs). The method was validated and applied to urine samples collected by three male volunteers after the administration of nandrolone-based formulations.Before the instrumental analysis, urine samples (<25 ml) were hydrolyzed with β-glucuronidase from Escherichia coli and extracted with n-pentane. Compounds of interest were purified through a single (for PT) or double (for 19-NE, 19-NA, A, and PD) liquid chromatographic step, to reduce the background noise and eliminate interferences that could have affect the accuracy of δ 13 C values. The limit of quantification (LOQ) of 2 ng/ml was ensured for both 19-NA and 19-NE. The 19-NE determination could be helpful in case of "unstable" urine samples, in late excretion phases or when coadministration with 5α-reductase inhibitors occur.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Detecting the abuse of 19‐norsteroids in doping controls: A new gas chromatography coupled to isotope ratio mass spectrometry method for the analysis of 19‐norandrosterone and 19‐noretiocholanolone

Iannella

Colamonici

Curcio

et al. 2020

Drug Testing and Analysis

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“…A simple method for sample pretreatment for 19‐NA by only one single HPLC purification with high isolation efficiency was developed by de la Torre and the co‐workers 19 . Podolskiy et al presented a procedure for determining the origin of 19‐NA with multistage pretreatment procedures including HPLC purification and acetylation 20 …”

Section: Introductionmentioning

confidence: 99%

Application of online two‐dimensional high‐performance liquid chromatography as purification procedure to determine the origin of 19‐norandrosterone in urine by gas chromatography–combustion–isotope ratio mass spectrometry

Wen

Zhu

Wang

et al. 2020

Drug Testing and Analysis

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19‐Norandrosterone (19‐NA) is the main metabolite of nandrolone and/or its precursors, which can be found naturally in human urine in trace amount. Gas chromatography–combustion–isotope ratio mass spectrometry (GC–C–IRMS) confirmation procedure can be used to identify a potential exogenous origin of 19‐NA in urine sample. Sample purification for GC–C–IRMS analysis is crucial to the whole confirmation procedure because the concentration of 19‐NA in the urine to be tested is very low. Online two‐dimensional high‐performance liquid chromatography (2D–HPLC) clean‐up procedure with high separation capacity is used to isolate and enrich 19‐NA as a sample pretreatment process. Linearity, lowest detectable concentration, uncertainty, and selectivity of the method are validated according to the World Anti‐doping Agency's (WADA) requirement. Isotope fractionation effect was not observed during the 2D‐HPLC purification process. The validated method provides a high efficient and convenient confirmation procedure to determine the origin of 19‐NA.

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Foodborne doping and supervision in sports

Chen

Cheng

et al. 2023

Food Science and Human Wellness

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Determination of the Origin of 19-Norandrosterone in Urine by Gas Chromatography–Isotope-Ratio Mass Spectrometry for Doping Control

Cited by 4 publications

References 12 publications

Detecting the abuse of 19‐norsteroids in doping controls: A new gas chromatography coupled to isotope ratio mass spectrometry method for the analysis of 19‐norandrosterone and 19‐noretiocholanolone

Detecting the abuse of 19‐norsteroids in doping controls: A new gas chromatography coupled to isotope ratio mass spectrometry method for the analysis of 19‐norandrosterone and 19‐noretiocholanolone

Application of online two‐dimensional high‐performance liquid chromatography as purification procedure to determine the origin of 19‐norandrosterone in urine by gas chromatography–combustion–isotope ratio mass spectrometry

Foodborne doping and supervision in sports

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