Determination of Residues of Cyromazine and Its Metabolite, Melamine, in Animal-Derived Food by Gas Chromatography−Mass Spectrometry with Derivatization

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• 作者：Xinle Zhu ; Shuhuai Wang ; Qi Liu ; Qian Xu ; Shixin Xu ; Huilan Chen
• 刊名：Journal of Agricultural and Food Chemistry
• 出版年：2009
• 出版时间：December 9, 2009
• 年：2009
• 卷：57
• 期：23
• 页码：11075-11080
• 全文大小：741K
• 年卷期：v.57,no.23(December 9, 2009)
• ISSN：1520-5118

文摘

A gas chromatography−mass spectrometric (GC-MS) method was established for the determination of cyromazine and its metabolite, melamine, in animal-derived food. Chicken and tilapia muscle samples were spiked with <sup>15sup>N<sub>3sub>-melamine, extracted with an acidic acetonitrile/water solution, and defatted with dichloromethane. Egg and milk samples were directly extracted with 3% trichloroacetic acid. The extracts were purified using mixed cation-exchange cartridges, derived with N,O-bis(trimethylsilyl)trifluoroacetamide, and detected by GC-MS. Cyromazine and melamine were quantified by external standard methods except for the determination of melamine in animal muscle, which used an internal standard method. Recoveries ranged from 75.0 to 110.0%, and relative standard deviations were <15.0%. In animal muscle the limits of quantification (LOQs) were 20 μg/kg and the limits of detection (LODs) were 10 μg/kg for cyromazine and melamine. In milk and eggs the LOQs were 10 μg/kg and the LODs were 5 μg/kg for both analytes.