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

Determination of Residues of Cyromazine and Its Metabolite, Melamine, in Animal-Derived Food by Gas Chromatography-Mass Spectrometry with Derivatization
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DOI:
10.1021/jf902771q
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发表时间:
2009-12-09
影响因子:
6.1
通讯作者:
Chen, Huilan
Chen, Huilan
中科院分区:
农林科学1区
文献类型:
--
作者:
Zhu, Xinle;Wang, Shuhuai;Chen, Huilan

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建立了动物源性食品中环丙嗪及其代谢物三聚氰胺的气相色谱-质谱(GC-MS)测定方法。鸡肉和罗非鱼肌肉样品中加入 (15)N(3)-三聚氰胺,用酸性乙腈/水溶液提取,并用二氯甲烷脱脂。鸡蛋和牛奶样品直接用3%三氯乙酸提取。使用混合阳离子交换柱纯化提取物,衍生自 N,O-双(三甲基甲硅烷基)三氟乙酰胺,并通过 GC-MS 检测。除动物肌肉中三聚氰胺的测定采用内标法外,灭蝇胺和三聚氰胺的定量均采用外标法。回收率范围为 75.0 至 110.0%,相对标准偏差为
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 (15)N(3)-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