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Quantitative detection of inhaled formoterol in human urine and relevance to doping control analysis.
Drug Test Anal. 2012 Jun; 4(6):449-54.DT

Abstract

Formoterol is a frequently prescribed β(2)-agonist used for the treatment of asthma. Due to performance-enhancing effects of some β(2) -agonists, formoterol appears on the prohibited list, published by the World Anti-doping Agency (WADA). Its therapeutic use is allowed but restricted to inhalation. Since the data on urinary concentrations originating from therapeutic use is limited, no discrimination can be made between use and misuse when a routine sample is found to contain formoterol. Therefore the urinary excretion of six volunteers after inhalation of 18 µg of formoterol was investigated. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of formoterol in 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, v/v). Analysis was performed using selected reaction monitoring after electrospray ionization. The method was linear in the range of 0.5-50 ng/ml. The limit of quantification (LOQ) was 0.5 ng/ml. The bias ranged between -1.0 and -6.8 %. Results for the urinary excretion show that formoterol could be detected for 72 h. The maximum urinary concentration detected was 8.5 ng/ml without and 11.4 ng/ml after enzymatic hydrolysis. Cumulative data showed that maximum 11.5% and 23% of the administered dose is excreted as parent drug within the first 12 h, respectively, non-conjugated and conjugated. Analysis of 82 routine doping samples, declared positive for formoterol during routine analysis, did not exhibit concentrations which could be attributed to misuse.

Authors+Show Affiliations

DoCoLab, UGent, Gent, Belgium. Koen.Deventer@UGent.beNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

22447497

Citation

Deventer, K, et al. "Quantitative Detection of Inhaled Formoterol in Human Urine and Relevance to Doping Control Analysis." Drug Testing and Analysis, vol. 4, no. 6, 2012, pp. 449-54.
Deventer K, Pozo OJ, Delbeke FT, et al. Quantitative detection of inhaled formoterol in human urine and relevance to doping control analysis. Drug Test Anal. 2012;4(6):449-54.
Deventer, K., Pozo, O. J., Delbeke, F. T., & Van Eenoo, P. (2012). Quantitative detection of inhaled formoterol in human urine and relevance to doping control analysis. Drug Testing and Analysis, 4(6), 449-54. https://doi.org/10.1002/dta.418
Deventer K, et al. Quantitative Detection of Inhaled Formoterol in Human Urine and Relevance to Doping Control Analysis. Drug Test Anal. 2012;4(6):449-54. PubMed PMID: 22447497.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitative detection of inhaled formoterol in human urine and relevance to doping control analysis. AU - Deventer,K, AU - Pozo,O J, AU - Delbeke,F T, AU - Van Eenoo,P, Y1 - 2012/03/22/ PY - 2011/10/15/received PY - 2011/12/25/revised PY - 2011/12/26/accepted PY - 2012/3/27/entrez PY - 2012/3/27/pubmed PY - 2012/11/6/medline SP - 449 EP - 54 JF - Drug testing and analysis JO - Drug Test Anal VL - 4 IS - 6 N2 - Formoterol is a frequently prescribed β(2)-agonist used for the treatment of asthma. Due to performance-enhancing effects of some β(2) -agonists, formoterol appears on the prohibited list, published by the World Anti-doping Agency (WADA). Its therapeutic use is allowed but restricted to inhalation. Since the data on urinary concentrations originating from therapeutic use is limited, no discrimination can be made between use and misuse when a routine sample is found to contain formoterol. Therefore the urinary excretion of six volunteers after inhalation of 18 µg of formoterol was investigated. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of formoterol in 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, v/v). Analysis was performed using selected reaction monitoring after electrospray ionization. The method was linear in the range of 0.5-50 ng/ml. The limit of quantification (LOQ) was 0.5 ng/ml. The bias ranged between -1.0 and -6.8 %. Results for the urinary excretion show that formoterol could be detected for 72 h. The maximum urinary concentration detected was 8.5 ng/ml without and 11.4 ng/ml after enzymatic hydrolysis. Cumulative data showed that maximum 11.5% and 23% of the administered dose is excreted as parent drug within the first 12 h, respectively, non-conjugated and conjugated. Analysis of 82 routine doping samples, declared positive for formoterol during routine analysis, did not exhibit concentrations which could be attributed to misuse. SN - 1942-7611 UR - https://www.unboundmedicine.com/medline/citation/22447497/Quantitative_detection_of_inhaled_formoterol_in_human_urine_and_relevance_to_doping_control_analysis_ L2 - https://doi.org/10.1002/dta.418 DB - PRIME DP - Unbound Medicine ER -