Scientific Publications by FDA Staff

J Agric Food Chem 2012 May 23;60(20):5084-8

Development of a Fast Screening and Confirmatory Method by Liquid Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry for Glucuronide-Conjugated Methyltestosterone Metabolite in Tilapia.

Amarasinghe K, Chu PS, Evans E, Reimschuessel R, Hasbrouck N, Jayasuriya H

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.