Development of a Method for the Detection and Confirmation of the alpha-2 Agonist Amitraz and Its Major Metabolite in Horse Urine
| Autor: | Andreas F. Lehner, J. Boyles, L. Dirikolu, W. Karpiesiuk, W. E. Woods, Charlie Hughes, F. C. Camargo, Thomas Tobin, Jeffrey M. Bosken, A. Troppmann, J. D. Harkins |
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| Rok vydání: | 2004 |
| Předmět: |
Spectrometry
Mass Electrospray Ionization Time Factors Toluidines Health Toxicology and Mutagenesis Electrospray ionization Metabolite Amidines Toxicology Mass spectrometry Gas Chromatography-Mass Spectrometry Analytical Chemistry chemistry.chemical_compound Animals Environmental Chemistry Selected ion monitoring Horses Adrenergic agonist Derivatization Amitraz Detection limit Chemical Health and Safety Chromatography Substance Abuse Detection chemistry Female Adrenergic alpha-Agonists |
| Zdroj: | Journal of Analytical Toxicology. 28:553-562 |
| ISSN: | 1945-2403 0146-4760 |
| Popis: | Amitraz (N'-(2,4-dimethylphenyl)-N-[[(2,4-dimethylphenyl)imino]methyl]-N-methyl-methanimidamide) is an alpha-2 adrenergic agonist used in veterinary medicine primarily as a scabicide- or acaricide-type insecticide. As an alpha-2 adrenergic agonist, it also has sedative/tranquilizing properties and is, therefore, listed as an Association of Racing Commissioners International Class 3 Foreign Substance, indicating its potential to influence the outcome of horse races. We identified the principal equine metabolite of amitraz as N-2,4-dimethylphenyl-N'-methylformamidine by electrospray ionization(+)-mass spectrometry and developed a gas chromatographic-mass spectrometric (GC-MS) method for its detection, quantitation, and confirmation in performance horse regulation. The GC-MS method involves derivatization with t-butyldimethylsilyl groups; selected ion monitoring (SIM) of m/z 205 (quantifier ion), 278, 261, and 219 (qualifier ions); and elaboration of a calibration curve based on ion area ratios involving simultaneous SIM acquisition of an internal standard m/z 208 quantifier ion based on an in-house synthesized d 6 deuterated metabolite. The limit of detection of the method is approximately 5 ng/mL in urine and is sufficiently sensitive to detect the peak urinary metabolite at 1 h post dose, following administration of amitraz at a 75-mg/horse intraveneous dose. |
| Databáze: | OpenAIRE |
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