Determination and Confirmation of Melamine Residues in Catfish, Trout, Tilapia, Salmon, and Shrimp by Liquid Chromatography with Tandem Mass Spectrometry

Abstract

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.

Potentiometric sensor based on molecularly imprinted polymer for determination of melamine in milk

“…Especially, the 2008 melamine-tainted-milk powder incident in China led to serious concern about melamine for food safety. Consequently, several methods have been developed for melamine detection in food, such as liquid chromatography coupled with mass spectrometry [25], solid phase extraction [26], ultraviolet spectrum, Raman spectroscopy and ion chromatogra- phy [27]. However, these methods require expensive apparatus and complicated pretreatment.…”

Simultaneous determination of melamine and related compounds by hydrophilic interaction liquid chromatography–electrospray mass spectrometry

“…Various techniques including HPLC-UV [10][11][12] or hydrophilic interaction liquid chromatography (HILIC)-UV [13], HPLC-MS [14][15][16][17][18][19][20][21][22][23][24], GC-MS [24][25][26], desorption ionization MS [27], CE [28][29][30], electrochemical method [31], etc., have been used to detect melamine or cyanuric acid. For the simultaneous determination of melamine and cyanuric acid, HPLC-MS [32] and MALDI-MS [33] were employed.…”

Application of Tandem Mass Spectrometry for Analyzing Melamine

“…The selected ion monitoring mode (SIM) was used for quantification and full scan mode for further identification (Litzau et at, 2008). LC-MS/MS has many applications in MEL analysis in food, feed and urine (Andersen et al, 2008;Somker & Krynitsky, 2008;Cheng et al, 2009a;Ibáñez et al, 2009;Zhang et al, 2010;Lutter et al, 2011) LC is suitable for the separation of polar MEL, and double stage mass (MS/MS) analysis provides high selectivity and sensitivity, with a reported detection limit range from 0.01 to 0.1 µg/g.…”