The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis (2023)

Ayotte, C., Romiguière, C., Fakirian, A., Flenker, U., Hebestreit, M., Piper, T. (2006). The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis. In W. Schänzer, H. Geyer, A. Gotzmann, & U. Mareck (Eds.), Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006 (pp. 277-287). (Recent advances in doping analysis; Vol. 14). Sport & Buch Strauß. http://www.sport-if.de/dokumente/Doping_Analysis/2006/articles/pp277-287.pdf

@inbook{f023e8ae3f5a478dad016ab8002c93dd,

title = "The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis",

abstract = "19-norandrosterone glucuronide (19-NA), main urinary metabolite of 19- nortestosterone, 19-norandrostenedione and 19-norandrostenediol, and minor metabolite of norethisterone , can also be produced, albeit in minute amounts, in males and females. Throughout pregnancy, 19-NA can be detected in urine samples at levels reaching approximately 15 ng/mL2. 19-nortestosterone is present in the intact boar; the consumption of meat-rich meal composed of non-castrated pig offal, although highly improbable, will lead to the excretion of 19-NA at levels exceeding the threshold. Adverse analytical findings are reported when the concentration of 19-NA is greater than 2 ng/mL taking into account the uncertainty of the measure; the threshold, introduced in 1998, is adjusted to the specific gravity of the specimen. Recently, the formation of 19-noretiocholanolone (19-NE) and 19-NA, the latter to a lesser extent, was reported in athlete's samples following incubation. Urine samples in which 19-demethylation activity was noted, were often very concentrated and turbid. This crucial observation, confirmed by two different groups, prompted the revision of the criteria for reporting adverse findings to include verification steps in the few samples showing the criteria of unstable urines. It is not possible to determine the endogenous or exogenous origin of urinary 19- norsteroids metabolites by the ratio of their 5a to 5{\ss} metabolites or by the ratio of the glucuro- and sulfoconjugates. The IRMS analysis may permit that differentiation. However, the reliable analysis of urinary 19-NA in trace amount by GC/C/IRMS was not possible without improving instrumental sensitivity and sample purification. We wish to report here, as a confirmation of the work already published by the Laboratory in Cologne, the results of the routinely applied GC/C/IRMS analysis of urine samples containing 19-NA in amount as low as 2 to 3 ng/mL in relatively low volume of urine sample. The IRMS analysis has been utilised to determine the endogenous origin of 19-NA present in athlete's samples as a result of 19-demethylation, thus confirming the occurrence of that reaction in athlete's urine samples. Einleitung (ge{\"a}ndert)",

keywords = "Biochemie, Doping, Dopingnachweis, Gaschromatographie, Leistungssport, Leistungssteigerung, Massenspektrometrie, Messverfahren, Norandrosteron, Sportmedizin, Untersuchungsmethode, Urin, Urinuntersuchung",

author = "C. Ayotte and C. Romigui{\`e}re and A. Fakirian and Ulrich Flenker and M. Hebestreit and Thomas Piper and Wilhelm Sch{\"a}nzer",

year = "2006",

language = "English",

series = "Recent advances in doping analysis",

publisher = "Sport & Buch Strau{\ss}",

pages = "277--287",

editor = "Wilhelm Sch{\"a}nzer and Hans Geyer and A. Gotzmann and Ute Mareck",

booktitle = "Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006",

note = "Cologne Workshop on Dope Analysis ; Conference date: 04-06-2006 Through 09-06-2006",

}

Ayotte, C, Romiguière, C, Fakirian, A, Flenker, U, Hebestreit, M, Piper, T 2006, The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis. in W Schänzer, H Geyer, A Gotzmann & U Mareck (eds), Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006. Recent advances in doping analysis, vol. 14, Sport & Buch Strauß, pp. 277-287, Cologne Workshop on Dope Analysis, Köln, Germany, 04.06.06. <http://www.sport-if.de/dokumente/Doping_Analysis/2006/articles/pp277-287.pdf>

The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis. / Ayotte, C.; Romiguière, C.; Fakirian, A. et al.

Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006. ed. / Wilhelm Schänzer; Hans Geyer; A. Gotzmann; Ute Mareck. Sport & Buch Strauß, 2006. p. 277-287 (Recent advances in doping analysis; Vol. 14).

Publication: Chapter in Book/Report/Conference proceeding › Conference contribution - Article for conference › Research

TY - CHAP

T1 - The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis

AU - Ayotte, C.

AU - Romiguière, C.

AU - Fakirian, A.

AU - Flenker, Ulrich

AU - Hebestreit, M.

AU - Piper, Thomas

AU - Schänzer, Wilhelm

N1 - Conference code: 24

PY - 2006

Y1 - 2006

N2 - 19-norandrosterone glucuronide (19-NA), main urinary metabolite of 19- nortestosterone, 19-norandrostenedione and 19-norandrostenediol, and minor metabolite of norethisterone , can also be produced, albeit in minute amounts, in males and females. Throughout pregnancy, 19-NA can be detected in urine samples at levels reaching approximately 15 ng/mL2. 19-nortestosterone is present in the intact boar; the consumption of meat-rich meal composed of non-castrated pig offal, although highly improbable, will lead to the excretion of 19-NA at levels exceeding the threshold. Adverse analytical findings are reported when the concentration of 19-NA is greater than 2 ng/mL taking into account the uncertainty of the measure; the threshold, introduced in 1998, is adjusted to the specific gravity of the specimen. Recently, the formation of 19-noretiocholanolone (19-NE) and 19-NA, the latter to a lesser extent, was reported in athlete's samples following incubation. Urine samples in which 19-demethylation activity was noted, were often very concentrated and turbid. This crucial observation, confirmed by two different groups, prompted the revision of the criteria for reporting adverse findings to include verification steps in the few samples showing the criteria of unstable urines. It is not possible to determine the endogenous or exogenous origin of urinary 19- norsteroids metabolites by the ratio of their 5a to 5ß metabolites or by the ratio of the glucuro- and sulfoconjugates. The IRMS analysis may permit that differentiation. However, the reliable analysis of urinary 19-NA in trace amount by GC/C/IRMS was not possible without improving instrumental sensitivity and sample purification. We wish to report here, as a confirmation of the work already published by the Laboratory in Cologne, the results of the routinely applied GC/C/IRMS analysis of urine samples containing 19-NA in amount as low as 2 to 3 ng/mL in relatively low volume of urine sample. The IRMS analysis has been utilised to determine the endogenous origin of 19-NA present in athlete's samples as a result of 19-demethylation, thus confirming the occurrence of that reaction in athlete's urine samples. Einleitung (geändert)

AB - 19-norandrosterone glucuronide (19-NA), main urinary metabolite of 19- nortestosterone, 19-norandrostenedione and 19-norandrostenediol, and minor metabolite of norethisterone , can also be produced, albeit in minute amounts, in males and females. Throughout pregnancy, 19-NA can be detected in urine samples at levels reaching approximately 15 ng/mL2. 19-nortestosterone is present in the intact boar; the consumption of meat-rich meal composed of non-castrated pig offal, although highly improbable, will lead to the excretion of 19-NA at levels exceeding the threshold. Adverse analytical findings are reported when the concentration of 19-NA is greater than 2 ng/mL taking into account the uncertainty of the measure; the threshold, introduced in 1998, is adjusted to the specific gravity of the specimen. Recently, the formation of 19-noretiocholanolone (19-NE) and 19-NA, the latter to a lesser extent, was reported in athlete's samples following incubation. Urine samples in which 19-demethylation activity was noted, were often very concentrated and turbid. This crucial observation, confirmed by two different groups, prompted the revision of the criteria for reporting adverse findings to include verification steps in the few samples showing the criteria of unstable urines. It is not possible to determine the endogenous or exogenous origin of urinary 19- norsteroids metabolites by the ratio of their 5a to 5ß metabolites or by the ratio of the glucuro- and sulfoconjugates. The IRMS analysis may permit that differentiation. However, the reliable analysis of urinary 19-NA in trace amount by GC/C/IRMS was not possible without improving instrumental sensitivity and sample purification. We wish to report here, as a confirmation of the work already published by the Laboratory in Cologne, the results of the routinely applied GC/C/IRMS analysis of urine samples containing 19-NA in amount as low as 2 to 3 ng/mL in relatively low volume of urine sample. The IRMS analysis has been utilised to determine the endogenous origin of 19-NA present in athlete's samples as a result of 19-demethylation, thus confirming the occurrence of that reaction in athlete's urine samples. Einleitung (geändert)

KW - Biochemie

KW - Doping

KW - Dopingnachweis

KW - Gaschromatographie

KW - Leistungssport

KW - Leistungssteigerung

KW - Massenspektrometrie

KW - Messverfahren

KW - Norandrosteron

KW - Sportmedizin

KW - Untersuchungsmethode

KW - Urin

KW - Urinuntersuchung

M3 - Conference contribution - Article for conference

T3 - Recent advances in doping analysis

SP - 277

EP - 287

BT - Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006

A2 - Schänzer, Wilhelm

A2 - Geyer, Hans

A2 - Gotzmann, A.

A2 - Mareck, Ute

PB - Sport & Buch Strauß

T2 - Cologne Workshop on Dope Analysis

Y2 - 4 June 2006 through 9 June 2006

ER -

Ayotte C, Romiguière C, Fakirian A, Flenker U, Hebestreit M, Piper T et al. The usefulness of GC/C/IRMS in determining the origin of low levels 19-NA - application in routine analysis. In Schänzer W, Geyer H, Gotzmann A, Mareck U, editors, Recent advances in doping analysis (14) : Proceedings of the Manfred Donike Workshop ; 24th Cologne Workshop on Dope Analysis 4th to 9th June 2006. Sport & Buch Strauß. 2006. p. 277-287. (Recent advances in doping analysis).