title: Determination of 17alpha-methyltestosterone in muscle tissues of tilapia, rainbow trout, and salmon using liquid chromatography-tandem mass spectrometry.
abstract: An analytical method was developed to quantitate and confirm the presence of 17alpha-methyltestosterone in the muscles of tilapia, rainbow trout, and salmon. The method employed two liquid-liquid partitioning steps and two solid-phase extraction columns for sample cleanup. The final extracts were analyzed on an isocratic reverse-phase liquid chromatography-tandem mass spectrometry system with atmospheric-pressure chemical ionization in the positive ion mode. The method was validated at levels from 0.40 to 1.6 ng/g, with MT-d3 used as an internal standard. The accuracy was between 100% and 110%, and coefficients of variation of <10% were obtained for all three fish species. Muscle tissues from dosed fish were also assayed to demonstrate the effectiveness of the method for recovering the parent drug.
authors.affiliation: Center for Veterinary Medicine, U.S. Food and Drug Administration, Laurel, Maryland 20708, USA. Pak.Chu@FDA.GOV
authors.forename: Pak-Sin
authors.initials: PS
authors.lastname: Chu
authors.forename: Mayda
authors.initials: M
authors.lastname: Lopez
authors.forename: Stan
authors.initials: S
authors.lastname: Serfling
authors.forename: Charlie
authors.initials: C
authors.lastname: Gieseker
authors.forename: Renate
authors.initials: R
authors.lastname: Reimschuessel
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis; D013058:Mass Spectrometry / Q000379:methods*; D008777:Methyltestosterone / Q000032:analysis*; D009132:Muscles / Q000737:chemistry*; D017686:Oncorhynchus mykiss; D012474:Salmon; D012680:Sensitivity and Specificity; D017210:Tilapia
chemical_list: D008777:Methyltestosterone