title: Use of methanol for the efficient extraction and analysis of melamine and cyanuric acid residues in dairy products and pet foods.
abstract: The recent worldwide shortage of acetonitrile has prompted the development of a new method using methanol as an alternative organic solvent in the extraction and liquid chromatographic analysis of melamine and cyanuric acid that may be present as contaminants in dairy products and pet foods. A simple extraction of melamine and cyanuric acid residues in fortified samples was successfully achieved, using a methanol-water mixture and analysis by isotopic dilution high-performance liquid chromatography-triple-quadrupole mass spectrometry (HPLC-MS/MS). A two-step centrifugation procedure was employed to remove matrix components from extracts. The separation of melamine and cyanuric acid was carried out on a Dionex Acclaim Trinity P1 column, with a methanol and ammonium acetate buffer used as the mobile phase. Excellent linearity was achieved for both the melamine and cyanuric acid calibrations. A variety of dairy products and pet foods were fortified with melamine and cyanuric acid at three levels, 1, 2.5, and 10 microg/g, producing recovery yields of 101-119% for melamine and 84-123% for cyanuric acid. The lower limit of quantification (LLOQ) of melamine was 0.03 microg/g for liquid milk and 0.05 microg/g for dry infant milk formula. The quantitative results were comparable with those derived from previous methods that have been proposed by the U.S. Food and Drug Administration for the screening of melamine and its analogues in foods.
authors.affiliation: Wadsworth Center, New York State Department of Health, Albany, New York 12201-0509, USA. btran@wadsworth.org
authors.forename: Buu N
authors.initials: BN
authors.lastname: Tran
authors.forename: Richard
authors.initials: R
authors.lastname: Okoniewski
authors.forename: Robin
authors.initials: R
authors.lastname: Storm
authors.forename: Robert
authors.initials: R
authors.lastname: Jansing
authors.forename: Kenneth M
authors.initials: KM
authors.lastname: Aldous
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D002417:Cattle; D005591:Chemical Fractionation / Q000379:methods*; D003611:Dairy Products / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis*; D000432:Methanol / Q000737:chemistry*; D014227:Triazines / Q000032:analysis*
chemical_list: D014227:Triazines; C004632:cyanuric acid; C011907:melamine; D000432:Methanol