title: Determination of residues of azamethiphos in salmon tissue by liquid chromatography with fluorescence detection.
abstract: A liquid chromatographic (LC) method with fluorescence detection (FLD) is described for determining residues of the pesticide azamethiphos (AZA) in salmon tissue. The sample is extracted with ethyl acetate, centrifuged, dehydrated with anhydrous sodium sulfate, evaporated, reconstituted in water, and defatted with hexane. The aqueous phase is passed through a C18 solid-phase extraction (SPE) column. The SPE column is eluted with methanol, and the eluate is evaporated to dryness and then taken up in 10% acetonitrile (ACN) in water. The analyte is determined by LC using a C18 column, ACN-H2O (32 + 68) mobile phase, and FLD with excitation at 230 nm and emission at 345 nm. Composited salmon tissues were fortified with AZA at 5, 10, 21, 42, and 83 ng/g or ppb (target level, X = 10 ng/g). Overall recoveries were 86%, with between-day variability of 5.3%. The method detection limit was calculated as 1.2 ppb AZA based on a 5 g sample. The limit of quantitation as determined empirically by this method is the lower limit of the standard curve, approximately 5 ppb.
authors.affiliation: U.S. Food and Drug Administration, Animal Drugs Research Center, Denver Federal Center, CO 80225-0087, USA.
authors.forename: A P
authors.initials: AP
authors.lastname: Pfenning
authors.forename: J E
authors.initials: JE
authors.lastname: Roybal
authors.forename: S B
authors.initials: SB
authors.lastname: Turnipseed
authors.forename: S A
authors.initials: SA
authors.lastname: Gonzales
authors.forename: J A
authors.initials: JA
authors.lastname: Hurlbut
mesh_terms: D000818:Animals; D002800:Cholinesterase Inhibitors / Q000032:analysis*; D002853:Chromatography, Liquid / Q000379:methods*; D007306:Insecticides / Q000032:analysis*; D063086:Organothiophosphates / Q000032:analysis; D010573:Pesticide Residues / Q000032:analysis*; D012474:Salmon / Q000378:metabolism*; D013050:Spectrometry, Fluorescence
chemical_list: D002800:Cholinesterase Inhibitors; D007306:Insecticides; D063086:Organothiophosphates; D010573:Pesticide Residues; C072763:azamethiphos