Determination and confirmation of melamine residues in catfish, trout, tilapia, salmon, and shrimp by liquid chromatography with tandem mass spectrometry.
Pet and food animal (hogs, chicken, and fish) feeds were recently found to be contaminated with melamine (MEL). A quantitative and confirmatory method is presented to determine MEL residues in edible tissues from fish fed this contaminant. Edible tissues were extracted with acidic acetonitrile, defatted with dichloromethane, and cleaned up using mixed-mode cation exchange solid-phase extraction cartridges. Extracts were analyzed by liquid chromatography with tandem mass spectrometry with hydrophilic interaction chromatography and electrospray ionization in positive ion mode. Fish and shrimp tissues were fortified with 10-500 microg/kg (ppb) of MEL with an average recovery of 63.8% (21.5% relative standard deviation, n = 121). Incurred fish tissues were generated by feeding fish up to 400 mg/kg of MEL or a combination of MEL and the related triazine cyanuric acid (CYA). MEL and CYA are known to form an insoluble complex in the kidneys, which may lead to renal failure. Fifty-five treated catfish, trout, tilapia, and salmon were analyzed after withdrawal times of 1-14 days. MEL residues were found in edible tissues from all of the fish with concentrations ranging from 0.011 to 210 mg/kg (ppm). Incurred shrimp and a survey of market seafood products were also analyzed as part of this study.
Andersen
Wendy C
WC
Animal Drugs Research Center and Denver District Laboratory, U.S. Food and Drug Administration, Denver Federal Center, P.O. Box 25087, Denver, Colorado 80225-0087, USA.
Turnipseed
Sherri B
SB
Karbiwnyk
Christine M
CM
Clark
Susan B
SB
Madson
Mark R
MR
Gieseker
Charles M
CM
Miller
Ron A
RA
Rummel
Nathan G
NG
Reimschuessel
Renate
R
D000821:Animal Feed / Q000032:analysis; D000818:Animals; D002853:Chromatography, Liquid; D005399:Fishes; D005506:Food Contamination / Q000032:analysis*; D007059:Ictaluridae; D012474:Salmon; D017747:Seafood / Q000032:analysis*; D012758:Shellfish / Q000032:analysis; D053719:Tandem Mass Spectrometry; D017210:Tilapia; D014227:Triazines / Q000032:analysis*; D014337:Trout
D014227:Triazines; C011907:melamine