Development of a fast screening and confirmatory method by liquid chromatography-quadrupole-time-of-flight mass spectrometry for glucuronide-conjugated methyltestosterone metabolite in tilapia.

Kande Amarasinghe, Pak-Sin Chu, Eric Evans, Renate Reimschuessel, Nicholas Hasbrouck, Hiranthi Jayasuriya

Center for Veterinary Medicine, Office of Research, U.S. Food and Drug Administration , Laurel, Maryland 20708, USA.

Journal of agricultural and food chemistry 2012 May 23

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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.

Citation

Kande Amarasinghe, Pak-Sin Chu, Eric Evans, Renate Reimschuessel, Nicholas Hasbrouck, Hiranthi Jayasuriya. Development of a fast screening and confirmatory method by liquid chromatography-quadrupole-time-of-flight mass spectrometry for glucuronide-conjugated methyltestosterone metabolite in tilapia. Journal of agricultural and food chemistry. 2012 May 23;60(20):5084-8