title: Analysis of sulfonamides, trimethoprim, fluoroquinolones, quinolones, triphenylmethane dyes and methyltestosterone in fish and shrimp using liquid chromatography-mass spectrometry.
abstract: A liquid chromatography-tandem mass spectrometry (LC-MS/MS) screening method is described for the detection and identification of 26 veterinary drugs in fish and other aquaculture products. The analytes include: 13 sulfonamides, trimethoprim, 3 fluoroquinolones, 3 quinolones, 3 triphenylmethane dyes, 2 leuco dye metabolites, and 1 hormone. In this method, tissue is mixed with EDTA-McIlvaine buffer, double-extracted with acetonitrile, p-toluenesulfonic (p-TSA) acid and N,N,N',N'-tetramethyl-p-phenylenediamine dihydrochloride (TMPD), and analyzed using LC-MS/MS. Inclusion of p-TSA and TMPD in the extraction procedure was critical for simultaneous analysis of dyes with the other groups of veterinary drugs. The proposed procedure was validated as both a quantitative analysis method and as a semi-quantitative screening method for multiple fish and shrimp matrices. The method was applied to eight types of fish (catfish, eel, pangasius, sablefish, tilapia, swai, salmon, and trout) and shrimp at the appropriate level of concern: 10ng/g for sulfonamides, trimethoprim, and quinolones, 5ng/g for fluoroquinolones, 1ng/g for dyes and their metabolites, and 0.4ng/g for methyltestosterone.
authors.affiliation: Animal Drugs Research Center, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States. Electronic address: joseph.storey@fda.hhs.gov.
authors.forename: Joseph M
authors.initials: JM
authors.lastname: Storey
authors.affiliation: Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Susan B
authors.initials: SB
authors.lastname: Clark
authors.affiliation: Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Aaron S
authors.initials: AS
authors.lastname: Johnson
authors.affiliation: Animal Drugs Research Center, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Wendy C
authors.initials: WC
authors.lastname: Andersen
authors.affiliation: Animal Drugs Research Center, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Sherri B
authors.initials: SB
authors.lastname: Turnipseed
authors.affiliation: Animal Drugs Research Center, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Jack J
authors.initials: JJ
authors.lastname: Lohne
authors.affiliation: Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Robert J
authors.initials: RJ
authors.lastname: Burger
authors.affiliation: Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Patrick R
authors.initials: PR
authors.lastname: Ayres
authors.affiliation: Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Justin R
authors.initials: JR
authors.lastname: Carr
authors.affiliation: Animal Drugs Research Center, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States; Denver Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, CO 80225-0087, United States.
authors.forename: Mark R
authors.initials: MR
authors.lastname: Madson
mesh_terms: D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D003445:Crustacea / Q000737:chemistry; D004350:Drug Residues / Q000032:analysis*; D005399:Fishes / Q000378:metabolism; D005506:Food Contamination / Q000032:analysis*; D017747:Seafood / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
keywords: Fluoroquinolones; LC–MS/MS; Multi-residue; Seafood; Sulfonamides; Triphenylmethane dyes