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Quantitative detection of inhaled salmeterol in human urine and relevance to doping control analysis

Koen Deventer UGent, Oscar Juan Pozo Mendoza UGent, Frans Delbeke UGent and Peter Van Eenoo UGent (2011) THERAPEUTIC DRUG MONITORING. 33(5). p.627-631
abstract
Salmeterol is a frequently prescribed beta(2)-agonist used for the treatment of asthma. Due to performance-enhancing effects of some beta(2)-agonists, salmeterol appears on the prohibited list published by the World Anti-Doping Agency and its therapeutic use is allowed but restricted to inhalation. Because the data on urinary concentrations originating from therapeutic use are limited, no discrimination can be made between use and abuse when a routine sample is found to contain salmeterol. Therefore, the urinary excretion of 100 mu g of inhaled salmeterol was investigated. A liquid chromatography-tandem mass spectrometry method was developed and validated for the quantification of urine samples. Sample preparation consists of an enzymatic hydrolysis of the urine samples followed by a liquid-liquid extraction at pH 9.5 with diethyl ether/isopropanol (5/1). Analysis was performed using selected reaction monitoring after electrospray ionization. The method was linear in the range of 0.5-50 ng/mL. The limits of quantification were 500 pg/mL. The inaccuracy ranged between 10.4% and -3.7%. Results show that salmeterol could be detected for 48 hours. The maximum urinary concentration detected was 1.27 ng/mL. Cumulative data showed that only 0.27% of the administered dose is excreted as parent drug within the first 12 hours. Analysis of 47 routine doping samples, declared to contain salmeterol during routine analysis, did not exhibit concentrations that could be considered originating from supratherapeutic doses.
Please use this url to cite or link to this publication:
author
organization
year
type
journalArticle (original)
publication status
published
subject
keyword
urine, mass spectrometry, doping, salmeterol, CHROMATOGRAPHY-MASS SPECTROMETRY, CLINICAL PHARMACOKINETICS, EQUINE URINE, BETA(2)-AGONISTS, CONFIRMATION, TERBUTALINE, METABOLISM, FENOTEROL, AGONISTS, detection
journal title
THERAPEUTIC DRUG MONITORING
Ther. Drug Monit.
volume
33
issue
5
pages
627 - 631
Web of Science type
Article
Web of Science id
000295083000008
JCR category
MEDICAL LABORATORY TECHNOLOGY
JCR impact factor
2.491 (2011)
JCR rank
8/32 (2011)
JCR quartile
2 (2011)
ISSN
0163-4356
DOI
10.1097/FTD.0b013e318229c5f4
language
English
UGent publication?
yes
classification
A1
copyright statement
I have transferred the copyright for this publication to the publisher
id
2045131
handle
http://hdl.handle.net/1854/LU-2045131
date created
2012-02-26 21:59:02
date last changed
2012-04-03 10:07:21
@article{2045131,
  abstract     = {Salmeterol is a frequently prescribed beta(2)-agonist used for the treatment of asthma. Due to performance-enhancing effects of some beta(2)-agonists, salmeterol appears on the prohibited list published by the World Anti-Doping Agency and its therapeutic use is allowed but restricted to inhalation. Because the data on urinary concentrations originating from therapeutic use are limited, no discrimination can be made between use and abuse when a routine sample is found to contain salmeterol. Therefore, the urinary excretion of 100 mu g of inhaled salmeterol was investigated. A liquid chromatography-tandem mass spectrometry method was developed and validated for the quantification of urine samples. Sample preparation consists of an enzymatic hydrolysis of the urine samples followed by a liquid-liquid extraction at pH 9.5 with diethyl ether/isopropanol (5/1). Analysis was performed using selected reaction monitoring after electrospray ionization. The method was linear in the range of 0.5-50 ng/mL. The limits of quantification were 500 pg/mL. The inaccuracy ranged between 10.4\% and -3.7\%. Results show that salmeterol could be detected for 48 hours. The maximum urinary concentration detected was 1.27 ng/mL. Cumulative data showed that only 0.27\% of the administered dose is excreted as parent drug within the first 12 hours. Analysis of 47 routine doping samples, declared to contain salmeterol during routine analysis, did not exhibit concentrations that could be considered originating from supratherapeutic doses.},
  author       = {Deventer, Koen and Pozo Mendoza, Oscar Juan and Delbeke, Frans and Van Eenoo, Peter},
  issn         = {0163-4356},
  journal      = {THERAPEUTIC DRUG MONITORING},
  keyword      = {urine,mass spectrometry,doping,salmeterol,CHROMATOGRAPHY-MASS SPECTROMETRY,CLINICAL PHARMACOKINETICS,EQUINE URINE,BETA(2)-AGONISTS,CONFIRMATION,TERBUTALINE,METABOLISM,FENOTEROL,AGONISTS,detection},
  language     = {eng},
  number       = {5},
  pages        = {627--631},
  title        = {Quantitative detection of inhaled salmeterol in human urine and relevance to doping control analysis},
  url          = {http://dx.doi.org/10.1097/FTD.0b013e318229c5f4},
  volume       = {33},
  year         = {2011},
}

Chicago
Deventer, Koen, Oscar Juan Pozo Mendoza, Frans Delbeke, and Peter Van Eenoo. 2011. “Quantitative Detection of Inhaled Salmeterol in Human Urine and Relevance to Doping Control Analysis.” Therapeutic Drug Monitoring 33 (5): 627–631.
APA
Deventer, K., Pozo Mendoza, O. J., Delbeke, F., & Van Eenoo, P. (2011). Quantitative detection of inhaled salmeterol in human urine and relevance to doping control analysis. THERAPEUTIC DRUG MONITORING, 33(5), 627–631.
Vancouver
1.
Deventer K, Pozo Mendoza OJ, Delbeke F, Van Eenoo P. Quantitative detection of inhaled salmeterol in human urine and relevance to doping control analysis. THERAPEUTIC DRUG MONITORING. 2011;33(5):627–31.
MLA
Deventer, Koen, Oscar Juan Pozo Mendoza, Frans Delbeke, et al. “Quantitative Detection of Inhaled Salmeterol in Human Urine and Relevance to Doping Control Analysis.” THERAPEUTIC DRUG MONITORING 33.5 (2011): 627–631. Print.