title: Simple quantitation of formoterol and 11-nor-Δ(9)-tetrahydrocannabinol-9-carboxylic acid in human urine by liquid chromatography-tandem mass spectrometry in doping control.
abstract: 11-nor-Δ(9)-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) and formoterol are newly revised prohibited threshold substances (150 ng/mL for THC-COOH and 40 ng/mL for formoterol) by the World Anti-Doping Agency (WADA). In continuation of our direct quantitation work of the prohibited threshold substances, direct LC-MS/MS methods combined with a simple sample preparation procedure have been developed and validated for the measurement of these two threshold substances in urine samples. After the enzymatic hydrolysis of urine samples, the resulting samples were diluted with acetonitrile and centrifuged. The supernatant was directly analyzed by LC-MS/MS using the selected reaction monitoring mode. The calibration curve range of the assay was ranged over 50-200% of the threshold value according to WADA guidelines. The limit of detection and limit of quantification were 6.1 and 18.4 ng/mL for THC-COOH and 2.0 and 6.2 ng/mL for formoterol, respectively. Intra- and inter-day precisions were between 2.08% and 7.28% and the accuracies ranged from 95.16% to 104.49%. The present methods were successfully applied to the analysis of the proficiency test samples.
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea.
authors: Kang Mi
authors: KM
authors: Lee
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea.
authors: Ho Jun
authors: HJ
authors: Kim
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea.
authors: Junghyun
authors: J
authors: Son
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea.
authors: Ju-Hyung
authors: JH
authors: Park
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea.
authors: Oh-Seung
authors: OS
authors: Kwon
authors: Doping Control Center, Korea Institute of Science and Technology, Hwarangno 14-gil 5, Seongbuk-gu, Seoul 136-791, Korea. Electronic address: jaeicklee@kist.re.kr.
authors: Jaeick
authors: J
authors: Lee
mesh_terms: D002853:Chromatography, Liquid / Q000379:methods*; D004300:Doping in Sports; D013759:Dronabinol / Q000031:analogs & derivatives* / Q000737:chemistry / Q000652:urine; D004983:Ethanolamines / Q000737:chemistry / Q000652:urine*; D000068759:Formoterol Fumarate; D006801:Humans; D057230:Limit of Detection; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D004983:Ethanolamines; C016780:11-nor-delta(9)-tetrahydrocannabinol-9-carboxylic acid; D013759:Dronabinol; D000068759:Formoterol Fumarate
keywords: Formoterol; Liquid chromatography; Quantitative analysis; THC-COOH; Tandem mass spectrometry