Miao Hong, Fan Sai, Wu Yong-Ning, Zhang Lei, Zhou Ping-Ping, Li Jing-Guang, Chen Hui-Jing, Zhao Yun-Feng
Department of Contaminant Monitoring and Control, Institute of Nutrition and Food Safety, Chinese Centre for Disease Control and Prevention, Beijing 100050, China.
Biomed Environ Sci. 2009 Apr;22(2):87-94. doi: 10.1016/S0895-3988(09)60027-1.
To develop an analytical method for simultaneously qualitative and quantitative determination of melamine and triazine-related by-products including ammelide, ammeline, and cyanuric acid in milk and milk products by gas chromatography-tandem mass spectrometry (GC-MS/MS).
Melamine and triazine-related by-products namely ammelide, ammeline and cyanuric acid in the samples were extracted in a solvent mixture of diethylamine, water, and acetonitrile (10:40:50, V/V/V). After centrifugation, an aliquot of the supernatant was evaporated to dryness under a gentle stream of nitrogen gas, and then melamine and triazine-related by-products were derivatized using BSTFA with 1% TMCS. The derivatives of melamine and its analogues were determined by gas chromatography/tandem mass spectrometry using multiple reactional monitoring (MRM) with 2, 6-Diamino-4-chloropyrimidine (DACP) being used as an internal standard.
The linear detectable ranges were from 0.004 mg/kg to 1.6 mg/kg for melamine, ammelide, ammeline, and cyanuric acid with a correlation coefficient no less than 0.999. The recovery rates of the four compounds in spiked blank milk powder at concentrations 0.5, 1, 2 mg/kg were between 61.4%-117.2%, and the relative standard deviation was no more than 11.5% (n=6). The detection limits of melamine, ammelide, ammeline and cyanuric acid in milk powder were 0.002 mg/kg with a ratio of signal to noise of 3.
This GC-MS/MS method for simultaneous determination of melamine, ammelide, ammeline, and cyanuric acid in milk and milk products is sensitive and specific.
建立一种气相色谱 - 串联质谱法（GC-MS/MS）同时定性和定量测定牛奶及奶制品中三聚氰胺以及包括三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸在内的三嗪相关副产物的分析方法。
样品中的三聚氰胺以及三嗪相关副产物三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸采用二乙胺、水和乙腈（10:40:50，V/V/V）的混合溶剂进行萃取。离心后，取上清液的一份等分试样在温和的氮气流下蒸发至干，然后使用含1%三甲基氯硅烷（TMCS）的N,O - 双（三甲基硅基）三氟乙酰胺（BSTFA）对三聚氰胺和三嗪相关副产物进行衍生化。以2,6 - 二氨基 - 4 - 氯嘧啶（DACP）为内标，采用多反应监测（MRM）模式通过气相色谱/串联质谱法测定三聚氰胺及其类似物的衍生物。
三聚氰胺、三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸的线性检测范围为0.004 mg/kg至1.6 mg/kg，相关系数不低于0.999。在浓度为0.5、1、2 mg/kg的加标空白奶粉中，这四种化合物的回收率在61.4% - 117.2%之间，相对标准偏差不超过11.5%（n = 6）。奶粉中三聚氰胺、三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸的检测限为0.002 mg/kg，信噪比为3。
这种用于同时测定牛奶及奶制品中三聚氰胺、三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸的GC-MS/MS方法灵敏且特异。
