Determination of Melamine Residues in Catfish Tissue by Triple Quadrupole LC-MS-MS with HILIC Chromatography
Wendy C. Andersen, Sherri B. Turnipseed, Christine M. Karbiwnyk, and Mark R. Madson U.S. Food and Drug Administration, Animal Drugs Research Center, Denver, CO
A triple quadrupole liquid chromatography tandem mass spectrometry method is presented for the quantitative determination and confirmation of melamine residues in catfish. Catfish tissue was extracted with 50:50 acetonitrile:water and 1 N hydrochloric acid and cleaned-up using Oasis® MCX solid phase extraction cartridges. Extracts were analyzed by LC-MS-MS with HILIC chromatography and electrospray ionization in positive ion mode. The precursor ion for melamine is m/z 127. Two product ion transitions were monitored at m/z 85 and 68 for quantification and confirmation. Catfish tissue was fortified at 10, 25, 50, 100, and 500 ng/g (ppb). The average recovery of melamine from fortified samples (n = 17) was 76.3 % with an RSD of 14.3 %.
INTRODUCTION
Pet food, animal feed, wheat gluten, and other protein-based food commodities were recently found to contain residues of melamine, an industrial chemical used in the manufacturing of plastics, flame retardants, and other products. It is not approved by the U.S. Food and Drug Administration for use in food or animal feed. Because animals may eat food contaminated with melamine residues, there is a need for analytical methods to determine melamine residues that may be present in animal tissues. This Laboratory Information Bulletin presents a method for the determination of trace levels of melamine in catfish muscle.
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