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Analysis of tretoquinol and its metabolites in human urine by liquid chromatography–tandem mass spectrometry
Author(s) -
Okano Masato,
Miyamoto Asami,
Sato Mitsuhiko,
Kageyama Shinji
Publication year - 2019
Publication title -
drug testing and analysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.065
H-Index - 54
eISSN - 1942-7611
pISSN - 1942-7603
DOI - 10.1002/dta.2714
Subject(s) - urine , chromatography , chemistry , glucuronide , metabolite , analyte , detection limit , liquid chromatography–mass spectrometry , tandem mass spectrometry , mass spectrometry , biochemistry
Tretoquinol (trimetoquinol), a β2‐agonist, has been explicitly listed on the World Anti‐Doping Agency Prohibited List 2019 since January 2019; however, it has been distributed as an antiasthmatic on the medical market. This study aimed to develop a liquid chromatography–tandem mass spectrometric method for the quantification of tretoquinol (free form plus glucuronide) in human urine for doping control purposes. An excretion study ( n = 6) of tretoquinol hydrochloride hydrate (6 mg) was performed, and urine samples were collected prior to oral administration and during the first 48 h, along with spot urine samples at 7 and 14 days after administration. All the urine samples were analysed using the developed method. The limit of detection for the developed method was 0.03 ng/mL. The inter‐day precision for the target analyte was excellent (2.7% to 9.2%), and the inter‐day accuracy of target analyte was −0.6% to −3.6%. In all subjects, tretoquinol (free form plus glucuronide conjugate) was identified up to 48 h after administration. The maximum concentrations were in the range of 12.4–78.8 ng/mL and the mean concentration was 55.3 ng/mL. The metabolites O‐ methylated tretoquinol, tretoquinol sulphate and O‐ methylated tretoquinol sulphate could be also identified in human urine after administration. The longest‐lasting urinary metabolite of tretoquinol currently known, O ‐methylated tretoquinol, is also likely to be a useful marker in doping controls.