title: Development of a fast screening and confirmatory method by liquid chromatography-quadrupole-time-of-flight mass spectrometry for glucuronide-conjugated methyltestosterone metabolite in tilapia.
abstract: This paper describes the development of a fast method to screen and confirm methyltestosterone 17-O-glucuronide (MT-glu) in tilapia bile. The method consists of solid-phase extraction (SPE) followed by high-performance liquid chromatography-mass spectrometry. The system used was an Agilent 6530 Q-TOF with an Agilent Jet stream electrospray ionization interface. The glucuronide detected in the bile was characterized as MT-glu by comparison with a chemically synthesized standard. MT-glu was detected in bile for up to 7 days after dosing. Semiquantification was done with matrix-matched calibration curves, because MT-glu showed signal suppression due to matrix effects. This method provides a suitable tool to monitor the illegal use of methyltestosterone in tilapia culture.
authors.affiliation: Center for Veterinary Medicine, Office of Research, U.S. Food and Drug Administration , Laurel, Maryland 20708, USA.
authors.forename: Kande
authors.initials: K
authors.lastname: Amarasinghe
authors.forename: Pak-Sin
authors.initials: PS
authors.lastname: Chu
authors.forename: Eric
authors.initials: E
authors.lastname: Evans
authors.forename: Renate
authors.initials: R
authors.lastname: Reimschuessel
authors.forename: Nicholas
authors.initials: N
authors.lastname: Hasbrouck
authors.forename: Hiranthi
authors.initials: H
authors.lastname: Jayasuriya
mesh_terms: D000818:Animals; D001646:Bile / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005506:Food Contamination / Q000032:analysis*; D020719:Glucuronides / Q000032:analysis* / Q000378:metabolism; D008297:Male; D013058:Mass Spectrometry / Q000379:methods; D008777:Methyltestosterone / Q000032:analysis* / Q000378:metabolism; D052616:Solid Phase Extraction; D017210:Tilapia
chemical_list: D020719:Glucuronides; D008777:Methyltestosterone