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Detection of inhaled clenbuterol in horse urine by GC/MS 2
Author(s) -
Van Eenoo P.,
Delbeke F. T.,
Deprez P.
Publication year - 2002
Publication title -
biomedical chromatography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.4
H-Index - 65
eISSN - 1099-0801
pISSN - 0269-3879
DOI - 10.1002/bmc.188
Subject(s) - clenbuterol , chemistry , chromatography , detection limit , urine , repeatability , mass spectrometry , derivatization , horse , gas chromatography–mass spectrometry , quantitative analysis (chemistry) , biochemistry , paleontology , biology
Clenbuterol, a β‐adrenergic agonist, is used in the treatment of recurrent airway obstruction in horses. It is prohibited by horse racing authorities, because of its stimulating and growth‐promoting properties. However, information on detection times of clenbuterol after administration by nebulization is lacking. In this study, a fast, sensitive quantitative GC‐MS 2 method for the detection of clenbuterol in urine was developed. Alkaline liquid–liquid extraction was followed by derivatization to a cyclic methyl boronate derivative and analysis on a Finnigan MAT GCQ instrument. Method validation showed good linearity in the range 0.1–2.0 ng/mL, excellent repeatability and specificity. The limit of quantitative detection of the method was 0.1 ng/ml. Different instrumental parameters of the ion trap mass spectrometer were changed to increase the number of diagnostic ions for the cyclic methyl boronate derivative of clenbuterol. The influence of these changes and their applicability within the requirements and the criteria for mass spectrometry set by the responsible regulatory bodies are discussed. Clenbuterol was administered via nebulization to five standardbred mares (0.4 µg/kg body weight). Analysis of the urine samples resulted in the detection of clenbuterol, as early as 2 h post administration and for up to 36 h post treatment. Generally, maximum urinary concentrations of 1.2 ng/mL were reached after 6–9 h. Copyright © 2002 John Wiley & Sons, Ltd.