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Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jun 01; 852(1-2):491-6.JC

Abstract

19-Norandrosterone sulfate (19-NAS) is the sulfoconjugated form of 19-norandrosterone (19-NA), the major metabolite of the steroid nandrolone. A sensitive and accurate liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay was developed for the direct measurement of 19-NAS in human urine samples. The method involved a quaternary amine SPE protocol and subsequently injection of the extract onto an analytical column (Uptisphere ODB, 150 mm x 3.0 mm, 5 microm) for chromatographic separation and mass spectrometry detection in negative electrospray ionisation mode. The sulfoconjugate of 19-NA was identified in urine by comparison of mass spectra and retention time with a reference substance. The limit of detection (LOD) and lowest limit of quantification (LLOQ) of 19-NAS were of 40 pg/mL and 200 pg/mL, respectively. For a nominal concentration of 2 ng/mL, recovery (94%), intra-day precision (2.7%), intra-assay precision (6.6%) and inter-assay precision (14.3%) were determined. Finally, this analytical method was applied for quantifying the concentration of 19-NAS in doping samples, using calibration curves (0.2-20 ng/mL) and the standard-addition method. The results show the feasibility of applying this LC-MS/MS assay as a complementary tool to detect misuse of nandrolone or nandrolone precursors.

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Authors+Show Affiliations

Strahm E
Laboratoire Suisse d'Analyse du Dopage, Institut Universitaire de Médecine Légale, Chemin des Croisettes 22, 1066 Epalinges, Switzerland.
Saudan C
No affiliation info available
Sottas PE
No affiliation info available
Mangin P
No affiliation info available
Saugy M
No affiliation info available

MeSH

Chromatography, LiquidEstranesHumansReference StandardsReproducibility of ResultsSensitivity and SpecificitySpectrometry, Mass, Electrospray IonizationTandem Mass Spectrometry

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

17321808

Citation

Strahm, Emmanuel, et al. "Direct Detection and Quantification of 19-norandrosterone Sulfate in Human Urine By Liquid Chromatography-linear Ion Trap Mass Spectrometry." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 852, no. 1-2, 2007, pp. 491-6.
Strahm E, Saudan C, Sottas PE, et al. Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2007;852(1-2):491-6.
Strahm, E., Saudan, C., Sottas, P. E., Mangin, P., & Saugy, M. (2007). Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 852(1-2), 491-6.
Strahm E, et al. Direct Detection and Quantification of 19-norandrosterone Sulfate in Human Urine By Liquid Chromatography-linear Ion Trap Mass Spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jun 1;852(1-2):491-6. PubMed PMID: 17321808.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Direct detection and quantification of 19-norandrosterone sulfate in human urine by liquid chromatography-linear ion trap mass spectrometry. AU - Strahm,Emmanuel, AU - Saudan,Christophe, AU - Sottas,Pierre-Edouard, AU - Mangin,Patrice, AU - Saugy,Martial, Y1 - 2007/02/15/ PY - 2006/10/25/received PY - 2007/01/25/revised PY - 2007/02/04/accepted PY - 2007/2/27/pubmed PY - 2007/8/2/medline PY - 2007/2/27/entrez SP - 491 EP - 6 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 852 IS - 1-2 N2 - 19-Norandrosterone sulfate (19-NAS) is the sulfoconjugated form of 19-norandrosterone (19-NA), the major metabolite of the steroid nandrolone. A sensitive and accurate liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay was developed for the direct measurement of 19-NAS in human urine samples. The method involved a quaternary amine SPE protocol and subsequently injection of the extract onto an analytical column (Uptisphere ODB, 150 mm x 3.0 mm, 5 microm) for chromatographic separation and mass spectrometry detection in negative electrospray ionisation mode. The sulfoconjugate of 19-NA was identified in urine by comparison of mass spectra and retention time with a reference substance. The limit of detection (LOD) and lowest limit of quantification (LLOQ) of 19-NAS were of 40 pg/mL and 200 pg/mL, respectively. For a nominal concentration of 2 ng/mL, recovery (94%), intra-day precision (2.7%), intra-assay precision (6.6%) and inter-assay precision (14.3%) were determined. Finally, this analytical method was applied for quantifying the concentration of 19-NAS in doping samples, using calibration curves (0.2-20 ng/mL) and the standard-addition method. The results show the feasibility of applying this LC-MS/MS assay as a complementary tool to detect misuse of nandrolone or nandrolone precursors. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/17321808/Direct_detection_and_quantification_of_19_norandrosterone_sulfate_in_human_urine_by_liquid_chromatography_linear_ion_trap_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(07)00108-0 DB - PRIME DP - Unbound Medicine ER -
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