Doping control analysis of four JWH-250 metabolites in equine urine by liquid chromatography-tandem mass spectrometry
| Autor: | Eric D. Vasilko, Youwen You, Mary A. Robinson, Rachel M. Proctor |
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| Rok vydání: | 2018 |
| Předmět: |
Detection limit
Chromatography Indoles Chemistry Cannabinoids Electrospray ionization Selected reaction monitoring Pharmaceutical Science Urine Anisoles Mass spectrometry Analytical Chemistry Triple quadrupole mass spectrometer Substance Abuse Detection JWH-250 Liquid chromatography–mass spectrometry Limit of Detection Tandem Mass Spectrometry Environmental Chemistry Animals Horses Spectroscopy Chromatography Liquid |
| Zdroj: | Drug testing and analysis. 11(5) |
| ISSN: | 1942-7611 |
| Popis: | JWH-250 is a synthetic cannabinoid. Its use is prohibited in equine sport according to the Association of Racing Commissioners International (ARCI) and the Federation Equestre Internationale (FEI). A doping control method to confirm the presence of four JWH-250 metabolites (JWH-250 4-OH-pentyl, JWH-250 5-OH-pentyl, JWH-250 5-OH-indole, and JWH-250 N-pentanoic acid) in equine urine was developed and validated. Urine samples were treated with acetonitrile and evaporated to concentrate the analytes prior to the analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The chromatographic separation was carried out using a Phenomenex Lux® 3 μm AMP column (150 x 3.0 mm). A triple quadrupole mass spectrometer was used for detection of the analytes in positive mode electrospray ionization using multiple reaction monitoring (MRM). The limits of detection, quantification, and confirmation for these metabolites were 25, 50, and 50 pg/mL, respectively. The linear dynamic range of quantification was 50-10000 pg/mL. Enzymatic hydrolysis indicated that JWH-250 4-OH-pentyl, JWH-250 5-OH-pentyl, and JWH-250 5-OH indole are highly conjugated whereas JWH-250 N-pentanoic acid is not conjugated. Relative retention time and product ion intensity ratios were employed as the criteria to confirm the presence of these metabolites in equine urine. The method was successfully applied to post-race urine samples collected from horses suspected of being exposed to JWH-250. All four JWH-250 metabolites were confirmed in these samples, demonstrating the method applicability for equine doping control analysis. |
| Databáze: | OpenAIRE |
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