title: Determination of melamine in milk and dairy products by high performance liquid chromatography.
abstract: A simple, precise, accurate, and validated reverse-phase HPLC method was developed for the determination of melamine in milk (pasteurized and UHT milk) and dairy products (powdered infant formula, fruit yogurt, soft cheese, and milk powder). Following extraction with acetonitrile:water (50:50, vol/vol), samples were purified by filter (0.45 μm), separated on a Nucleosil C8 column (4.6 mm × 250 mm, 3 μm) with acetonitrile:10 mmol/L sodium L-octane sulfonate (pH 3.1; 15:85, vol/vol) as mobile phase at a flow rate of 1 mL/min, and determined by a photodiode array detector. A linear calibration curve was obtained in the concentration range from 0.05 to 5 mg/kg. Milk and dairy products were fortified with melamine at 4 levels producing average recovery yields of 95 to 109%. The limits of detection and quantification of melamine were 35 to 110 and 105 to 340 μg/kg, respectively. The method was then used to analyze 300 samples of milk and dairy products purchased from major retailers in Turkey. Melamine was not found in infant formulas and pasteurized UHT milk, whereas 2% of cheese, 8% of milk powder, and 44% of yogurt samples contained melamine at the 121, 694±146, and 294±98 μg/kg levels, respectively. These findings were below the limits set by the Codex Alimentarius Commission and European Union legislation. This is the first study to confirm the existence of melamine in milk and dairy products in Turkey. Consumption of foods containing these low levels of melamine does not constitute a health risk for consumers.
authors.affiliation: Department of Pharmacology and Toxicology, Ankara University, Faculty of Veterinary Medicine, Ankara, Turkey 06110. filazi@veterinary.ankara.edu.tr
authors.forename: A
authors.initials: A
authors.lastname: Filazi
authors.forename: U T
authors.initials: UT
authors.lastname: Sireli
authors.forename: H
authors.initials: H
authors.lastname: Ekici
authors.forename: H Y
authors.initials: HY
authors.lastname: Can
authors.forename: A
authors.initials: A
authors.lastname: Karagoz
mesh_terms: D000818:Animals; D002417:Cattle; D002611:Cheese / Q000032:analysis; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003611:Dairy Products / Q000032:analysis*; D005506:Food Contamination / Q000032:analysis; D006801:Humans; D007223:Infant; D041943:Infant Formula / Q000737:chemistry; D008892:Milk / Q000737:chemistry*; D014227:Triazines / Q000032:analysis*; D014421:Turkey; D015014:Yogurt / Q000032:analysis
chemical_list: D014227:Triazines; C011907:melamine