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- E-ISSN 2093-8950
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Identification of Nandrolone and its Metabolite 5α-Estran-3β, 17α-Diol in Horse Urine after Chemical Derivatization by Liquid Chromatography Tandem Mass Spectrometry
Mass Spectrometry Letters / Mass Spectrometry Letters, (P)2233-4203; (E)2093-8950
2017, v.8 no.4, pp.90-97
https://doi.org/10.5478/MSL.2017.8.4.90
(National Dope Testing Laboratory)
(Anti-Doping Laboratory)
(Anti-Doping Laboratory)
Dubey,
S., &
Beotra,
A.
(2017). Identification of Nandrolone and its Metabolite 5α-Estran-3β, 17α-Diol in Horse Urine after Chemical Derivatization by Liquid Chromatography Tandem Mass Spectrometry. Mass Spectrometry Letters, 8(4), 90-97, https://doi.org/10.5478/MSL.2017.8.4.90
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Abstract
Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry (LC/MSn) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, 5α-estrane-3β, 17α-diol exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in LC-ESI-MSn analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.
- keywords
- Liquid chromatography tandem mass spectrometry, nandrolone, chemical derivatization, Horse urine
Reference
1
International Federation of Horseracing Authorities. (2016). International agreement on breeding, racing and wagering. http://www.horseracingintfed.com/resources/2015Agreement.pdf.
2
Roig, M. (2007). . J. Anal. Chim. Acta, 586, 184-.
3
Takeda, A. (2001). . J. Chromatogr. B, 758, 235-.
4
Williams, R. B. (2001). (-). Proc. 13th Int. Conf. Racing Anal. Vet. R&W publications.
5
Hill, D. W. (2003). (-). Proc. 14th Int. Conf. Racing Anal. Vet. R&W publications.
6
Thieme, D. (2003). . Anal. Chim. Acta, 492, 171-.
7
Albert, P. H. (2004). (-). Proc. 15th Int. Conf. Racing Anal. Vet. R&W publications.
8
Guan, F. (2005). . J. Chromatogr. B, 829, 56-.
9
Stewart, R. T. (2009). . J. Steroid Biochem. Mol. Bio, 117, 152-.
10
Houghton, E. (1988). . Analyst, 113, 1179-.
11
Snow, D. H. (1982). . J. Equine Vet. Sci, 14, 224-.
12
Wynne, P. M. (2000). The application of SPE to veterinary drug abuse:Racing Analytical Services Limited.
13
G. N. W. Leung. (2005). . J. Chromatogr. B, 825, 47-56.
14
Makin, H. L. J. (2010). . J. Steroid Analysis, Springer, , -.
15
Yu, N. H. (2008). . J. Chromatogr. A, 1189, 426-.
16
Stanley, S. M. R. (2006). . J. Chromatogr. B, 836, 1-.
17
Touber, M. E. (2007). . Anal. Chim. Acta, 586, 137-.
18
Wong, C. H. F. (2011). . J. Anal. Chim. Acta, 697, 48-.
19
Kwok, W. H. (2010). . J. Chromatogr. A, 1217, 3289-.
20
Eenoo, P. V. (2002). Mass spectrometric detection of doping substances:Ghent University.
21
Pozo, O. J. (2008). . Trends Anal. Chem, 27, 657-.
22
Stanley, S. M. R. (2007). . J. Chromatogr. B, 848, 292-.
23
Ho, E. N. M. (2006). . J. Chromatogr. A, 1120, 38-.
24
Guan, F. (2010). . J. Mass Spectrom, 45, 1270-.
25
Deng, P. (2012). . Bioanalysis, 4, 49-.
26
Wong, C. H. F. (2012). . J. Chromatogr. A, 1232, 257-.
27
Athanasiadou, I. (2013). . Trends Anal. Chem, 42, 137-.
28
International Federation of Horseracing Authorities. (2016). International agreement on breeding, racing and wagering. http://www.horseracingintfed.com/resources/2015Agreement.pdf.
29
Association of Racing Commissioners International. (2017). Model Rules of Racing Version 8.0. http://arci.blob.core.windows.net/webdocs/2017%2007%20Model_Rules_V8.0.pdf.
30
Pozo, O. J. (2007). . J. Mass Spectrom, 42, 497-.
31
Thevis, M. (2007). . Anal. Bioanal. Chem, 388, 1351-.
32
Yamashita, K. (2007). . Steroids, 72, 50-.
33
Yamashita, K. (2007). . J. Chromatogr. A, 1173, 120-.
34
Yamashita, K. (2009). . J. Mass Spectrom. Soc. Jpn, 57, 75-.
- Submission Date
- 2017-04-20
- Revised Date
- 2017-07-21
- Accepted Date
- 2017-09-14
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