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Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques.
J Chromatogr Sci. 2013 May-Jun; 51(5):436-45.JC

Abstract

This study demonstrates the development of a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS-MS) assay to detect clenbuterol in human urine and the comparison of this method with GC-MS techniques and gas chromatography-high resolution mass spectrometry (GC-HRMS) techniques. Urine samples were hydrolyzed with β-glucuronidase, extracted with methyl tert-butyl ether and dried under nitrogen. The derivative reagent was N-methyl-N-(trimethylsilyl)-trifluoroacetamide with NH4I and was analyzed by GC-MS, GC-MS-MS and GC-HRMS. A validation study was conducted by GC-MS-MS. The analyses of clenbuterol using different mass spectrometric techniques were compared. The limit of detection (LOD) for clenbuterol in human urine was 2 ng/mL by GC-MS (selected ion monitoring mode: SIM mode), 0.06 ng/mL by GC-HRMS and 0.03 ng/mL by GC-MS-MS, respectively, while the LOD by GC-HRMS was 0.06. With GC-MS-MS, the intra-assay and inter-assay precisions were less than 15%, the recoveries were 86 to 112% and the linear range was 0.06 to 8.0 ng/mL. The GC-MS under SIM mode can be used as a screening tool to detect clenbuterol at trace levels in human urine. The GC-MS-MS and GC-HRMS methods can confirm clenbuterol when its concentration is below 2 ng/mL. The results demonstrate that the GC-MS-MS method is quite sensitive, specific and reliable for the detection of clenbuterol in doping analysis.

Authors+Show Affiliations

National Anti-doping Laboratory, China Anti-Doping Agency, 1st Anding Road, ChaoYang District, Beijing 100029, P. R. China. yangsheng@chinada.cnNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

23042839

Citation

Yang, Sheng, et al. "Detection of Clenbuterol at Trace Levels in Doping Analysis Using Different Gas Chromatographic-mass Spectrometric Techniques." Journal of Chromatographic Science, vol. 51, no. 5, 2013, pp. 436-45.
Yang S, Liu X, Xing Y, et al. Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques. J Chromatogr Sci. 2013;51(5):436-45.
Yang, S., Liu, X., Xing, Y., Zhang, D., Wang, S., Wang, X., Xu, Y., Wu, M., He, Z., & Zhao, J. (2013). Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques. Journal of Chromatographic Science, 51(5), 436-45. https://doi.org/10.1093/chromsci/bms160
Yang S, et al. Detection of Clenbuterol at Trace Levels in Doping Analysis Using Different Gas Chromatographic-mass Spectrometric Techniques. J Chromatogr Sci. 2013 May-Jun;51(5):436-45. PubMed PMID: 23042839.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Detection of clenbuterol at trace levels in doping analysis using different gas chromatographic-mass spectrometric techniques. AU - Yang,Sheng, AU - Liu,Xin, AU - Xing,Yanyi, AU - Zhang,Dapeng, AU - Wang,Shan, AU - Wang,Xiaobing, AU - Xu,Youxuan, AU - Wu,Moutian, AU - He,Zhenwen, AU - Zhao,Jian, Y1 - 2012/10/05/ PY - 2012/10/9/entrez PY - 2012/10/9/pubmed PY - 2013/9/10/medline SP - 436 EP - 45 JF - Journal of chromatographic science JO - J Chromatogr Sci VL - 51 IS - 5 N2 - This study demonstrates the development of a gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS-MS) assay to detect clenbuterol in human urine and the comparison of this method with GC-MS techniques and gas chromatography-high resolution mass spectrometry (GC-HRMS) techniques. Urine samples were hydrolyzed with β-glucuronidase, extracted with methyl tert-butyl ether and dried under nitrogen. The derivative reagent was N-methyl-N-(trimethylsilyl)-trifluoroacetamide with NH4I and was analyzed by GC-MS, GC-MS-MS and GC-HRMS. A validation study was conducted by GC-MS-MS. The analyses of clenbuterol using different mass spectrometric techniques were compared. The limit of detection (LOD) for clenbuterol in human urine was 2 ng/mL by GC-MS (selected ion monitoring mode: SIM mode), 0.06 ng/mL by GC-HRMS and 0.03 ng/mL by GC-MS-MS, respectively, while the LOD by GC-HRMS was 0.06. With GC-MS-MS, the intra-assay and inter-assay precisions were less than 15%, the recoveries were 86 to 112% and the linear range was 0.06 to 8.0 ng/mL. The GC-MS under SIM mode can be used as a screening tool to detect clenbuterol at trace levels in human urine. The GC-MS-MS and GC-HRMS methods can confirm clenbuterol when its concentration is below 2 ng/mL. The results demonstrate that the GC-MS-MS method is quite sensitive, specific and reliable for the detection of clenbuterol in doping analysis. SN - 1945-239X UR - https://www.unboundmedicine.com/medline/citation/23042839/Detection_of_clenbuterol_at_trace_levels_in_doping_analysis_using_different_gas_chromatographic_mass_spectrometric_techniques_ L2 - https://academic.oup.com/chromsci/article-lookup/doi/10.1093/chromsci/bms160 DB - PRIME DP - Unbound Medicine ER -